天堂网亚洲,天天操天天搞,91视频高清,菠萝蜜视频在线观看入口,美女视频性感美女视频,95丝袜美女视频国产,超高清美女视频图片

Home Cart 0 Sign in  

[ CAS No. 867130-58-3 ] {[proInfo.proName]}

,{[proInfo.pro_purity]}
Cat. No.: {[proInfo.prAm]}
Chemical Structure| 867130-58-3
Chemical Structure| 867130-58-3
Structure of 867130-58-3 * Storage: {[proInfo.prStorage]}

Please Login or Create an Account to: See VIP prices and availability

Cart0 Add to My Favorites Add to My Favorites Bulk Inquiry Inquiry Add To Cart

Search after Editing

* Storage: {[proInfo.prStorage]}

* Shipping: {[proInfo.prShipping]}

Quality Control of [ 867130-58-3 ]

Related Doc. of [ 867130-58-3 ]

Alternatived Products of [ 867130-58-3 ]
Product Citations

Product Details of [ 867130-58-3 ]

CAS No. :867130-58-3 MDL No. :MFCD08437486
Formula : C5H4N2O3 Boiling Point : No data available
Linear Structure Formula :- InChI Key :PSMIHCDKMNXTAY-UHFFFAOYSA-N
M.W : 140.10 Pubchem ID :12376265
Synonyms :

Safety of [ 867130-58-3 ]

Signal Word:Warning Class:
Precautionary Statements:P261-P280-P305+P351+P338 UN#:
Hazard Statements:H302-H315-H319-H332-H335 Packing Group:
GHS Pictogram:

Application In Synthesis of [ 867130-58-3 ]

* All experimental methods are cited from the reference, please refer to the original source for details. We do not guarantee the accuracy of the content in the reference.

  • Downstream synthetic route of [ 867130-58-3 ]

[ 867130-58-3 ] Synthesis Path-Downstream   1~14

  • 1
  • [ 867130-58-3 ]
  • [ 504-30-3 ]
  • 2
  • [ 21427-85-0 ]
  • [ 867130-58-3 ]
  • 4
  • [ 54709-94-3 ]
  • [ 867130-58-3 ]
YieldReaction ConditionsOperation in experiment
87% With potassium permanganate; sulfuric acid; at 45℃; for 1.0h; Example 386-Oxo-1,6-dihydro-pyridazine-4-carboxylic acid The title compound from Example 37 (0.90 g, 8.2 mmol) was stirred in concentrated sulfuric acid (13 mL) and heated to 45 C. Potassium permanganate (3.6 g, 12 mmol) was added portion wise over 30 min to avoid letting the temperature rise. The reaction was allowed to stir for a further 30 min at 45 C. The reaction was then cooled to room temperature and ice was added to the reaction mixture. The resulting precipitate was collected by vacuum filtration, washing with cold water and diethyl ether to give 0.98 g (87%) of the title compound as the a pale green solid.1H NMR (300 MHz, CDCl3): delta (ppm) 13.39 (broad s, 1H), 8.12 (s, 1H), 7.22 (s, 1H).
87% With potassium permanganate; sulfuric acid; at 45℃; for 1.0h; 6-Oxo-l,6-dihydro-pyridazine-4-carboxylic acidThe title compound from Example 18.2 (0.90 g, 8.17 mmol) was stirred in concentrated sulfuric acid (13 mL) and heated to 45 0C. Potassium permanganate (3.6 g, 12.25 mmol) was added portion wise over 30 min to avoid letting the temperature rise. The reaction was allowed to stir for a further 30 min at 45 0C. The reaction was then cooled to r.t. and ice was added to the reaction mixture. The resulting precipitate was collected by vacuum filtration, washing with cold water and diethyl ether to give 0.978 g (87%) of the title compound as the a pale green solid. 1H NMR (300 MHz, CDCl3) delta 13.39 (br, IH), 8.12 (s, IH), 7.22 (s, IH).
77% Example 306-Oxo-1,6-dihydro-pyridazine-4-carboxylic acid To a stirred solution of the title compound of Example 29 (4.4 g, 40 mmol) in concentrated sulphuric acid (80 mL), potassium dichromate (18 g, 61 mmol) was added in small quantities at 50-60 C. as a finely ground powder. The starting material was added to the mixture within 20 min. Stirring was continued for a further 10 min at 60 C., then the viscous green mixture was poured on crushed ice. The solid powder, which separated, was collected, washed with cold water and dried to give the title compound (4.5 g, 77%).1H NMR (400 MHz, (CD3)2SO): delta (ppm) 7.22 (s, 3H), 8.13 (s, 1H), 13.38 (s, broad, 1H).
77% With dipyridinium dichromate; sulfuric acid; at 50 - 60℃; for 0.5h; Step 14B: 6-Oxo-1H-pyridazine-4-carboxylic acid; To a stirred solution of the subtitle compound of Step 14A (4.4 g, 40 mmol) in concentrated sulphuric acid (80 mL), potassium dichromate (18 g, 61 mmol) was added in small quantities at 50-60 C. as a finely ground powder. The starting material was added to the mixture within 20 min. Stirring was continued for a further 10 min at 60 C., then the viscous green mixture was poured on crushed ice. The solid powder, which separated, was collected, washed with cold water and dried to give the subtitle compound (4.5 g, 77%).1H NMR (400 MHz, (CD3)2SO): delta 7.22 (s, 3H), 8.13 (s, 1H), 13.38 (s, broad, 1H).
77% With potassium dichromate; sulfuric acid; at 50 - 60℃; for 0.5h; Step 10B: 6-Oxo-1,6-dihydropyridazine-4-carboxylic acid; To a stirred solution of the subtitle compound of Step 10A (4.4 g, 40 mmol) in concentrated sulphuric acid (80 mL), potassium dichromate (18 g, 61 mmol) was added in small quantities at 50-60 C. as a finely ground powder. The starting material was added to the mixture within 20 min. Stirring was continued for 10 min at 60 C., the viscous green mixture was poured on crushed ice. The solids were filtered off and washed with cold water. After drying in vacuo the subtitle compound was isolated (4.5 g, 77%).1H NMR (400 MHz, DMSO-d6): delta 7.22 (s, 3H), 8.13 (s, 1H), 13.38 (s, broad, 1H).
77% With potassium dichromate; sulfuric acid; at 50 - 60℃; for 0.5h; Step 7B: 6-Oxo-1,6-dihydropyridazine-4-carboxylic Acid To a stirred solution of the subtitle compound of Step 7A (4.4 g, 40 mmol) in concentrated sulphuric acid (80 mL), potassium dichromate (18 g, 61 mmol) was added in small quantities at 50-60 C. as a finely ground powder. The starting material was added to the mixture within 20 min. Stirring was continued for a further 10 min at 60 C., then the viscous green mixture was poured on crushed ice. The solid powder, which separated, was collected, washed with cold water and dried to give the subtitle compound (4.5 g, 77%).1H NMR (400 MHz, (CD3)2SO): delta 7.22 (s, 3H), 8.13 (s, 1H), 13.38 (s, broad, 1H).
77% With potassium dichromate; sulfuric acid; at 60℃; for 0.166667h; Step 13B: 6-Oxo-1,6-dihydropyridazine-4-carboxylic acid To a stirred solution of the subtitle compound of Step 13A (4.4 g, 40 mmol) in concentrated sulphuric acid (80 mL), potassium dichromate (18 g, 61 mmol) was added in small quantities at 50-60 C. as a finely ground powder. The starting material was added to the mixture within 20 min. Stirring was continued for a further 10 min at 60 C., the viscous green mixture was poured on crushed ice. The solids were filtered off and washed with cold water. After drying in vacuo the subtitle compound was isolated (4.5 g, 77%). 1H NMR (400 MHz, (CD3)2SO): delta 7.22 (s, 3H), 8.13 (s,1H), 13.38 (s, broad, 1H).

  • 5
  • [ 867130-58-3 ]
  • [ 64-17-5 ]
  • [ 21427-85-0 ]
YieldReaction ConditionsOperation in experiment
83% Step 14C: Ethyl 6-oxo-1H-pyridazine-4-carboxylate; The compound of Step 14B was dissolved in EtOH (10 mL) and concentrated H2SO4 (4.2 mL) was added and then heated at reflux for 5 h. The reaction mixture was cooled, concentrated in vacuo and basified with saturated Na2CO2. After filtration, the aqueous phase was extracted with EtOAc, dried over anhydrous Na2SO4, filtered and concentrated to give the subtitle product (83%).1H NMR (400 MHz, CD3OD): delta 8.27 (d, 1H), 7.42 (d, 1H), 4.40 (q, 2H), 1.39 (t, 3H).
83% Step 10C: Ethyl 6-oxo-1,6-dihydropyridazine-4-carboxylate; The subtitle compound of step 10B was dissolved in EtOH (10 mL) and concentrated H2SO4 (4.2 mL) was added and then heated at reflux for 5 hours. The reaction mixture was cooled, concentrated in vacuo and basified with saturated Na2CO3. After filtration, the aqueous phase was extracted with ethyl acetate, dried over anhydrous Na2SO4, filtered and concentrated to give the subtitle compound (83%).1H NMR (400 MHz, MeOH-d4): delta 8.27 (d, 1H), 7.42 (d, 1H), 4.40 (q, 2H), 1.39 (t, 3H).
83% Step 7C: Ethyl 6-oxo-1,6-dihydropyridazine-4-carboxylate The subtitle product of Step 7B was dissolved in EtOH (10 mL) and concentrated H2SO4 (4.2 mL) was added and then heated at reflux for 5 hours. The reaction mixture was cooled, concentrated in vacuo and basified with saturated Na2CO3. After filtration, the aqueous phase was extracted with EtOAc, dried over anhydrous Na2SO4, filtered and concentrated to give the subtitle compound (83%).1H NMR (400 MHz, CD3OD): delta 8.27 (d, 1H), 7.42 (d, 1H), 4.40 (q, 2H), 1.39 (t, 3H).
83% With sulfuric acid; for 5.0h;Heating / reflux; Step 13C: Ethyl 6-oxo-1,6-dihydropyridazine-4-carboxylate The compound of step 13B was dissolved in EtOH (10 mL) and concentrated H2SO4 (4.2 mL) was added and then heated at reflux for 5 hours. The reaction mixture was cooled, concentrated in vacuo and basified with saturated Na2CO3. After filtration, the aqueous phase was extracted with ethyl acetate, dried over anhydrous Na2SO4, filtered and concentrated to give the subtitle compound (83%). 1H NMR (400 MHz, CD3OD): delta 8.27 (d, 1H), 7.42 (d, 1H), 4.40 (q, 2H), 1.39 (t, 3H).
With acetyl chloride; at 75℃; Example 39.1<strong>[867130-58-3]6-Oxo-1,6-dihydro-pyridazine-4-carboxylic acid</strong> ethyl ester The title compound from Example 38 (1.0 g, 7.13 mmol) was added to a solution of ethanol (16 mL) and acetyl chloride (4 mL) and the resulting suspension was heated to 75 C. and stirred overnight. The reaction mixture was concentrated, diluted with water and extracted with dichloromethane. The organic phase was dried over sodium sulfate, filtered and concentrated to give the title compound.1H NMR (300 MHz, CDCl3): delta (ppm) 10.91 (broad s, 1H), 8.26 (s, 1H), 7.53 (s, 1H), 4.43 (q, 2H), 1.40 (t, 3H).
With acetyl chloride; at 75℃; 6-Oxo-l,6-dihydro-pyridazine-4-carboxylic acid ethyl esterThe title compound from Example 18.3 (1.0 g, 7.13 mmol) was added to a solution of ethanol (16 mL) and acetyl chloride (4 mL) and the resulting suspension was heated to 75 C and stirred overnight. The reaction mixture was concentrated, diluted with water and extracted with dichloromethane. The organic phase was dried over sodium sulfate, filtered and concentrated to give the title compound.1H NMR (300 MHz, CDCl3) delta 10.91 (br, IH), 8.26 (s, IH), 7.53 (s, IH), 4.43 (q, 2H), 1.40 (t, 3H).

  • 6
  • [ 412301-44-1 ]
  • [ 867130-58-3 ]
  • 7
  • [ 5472-38-8 ]
  • [ 867130-58-3 ]
  • 8
  • [ 867130-58-3 ]
  • 6-chloropyridazine-4-carbonyl chloride [ No CAS ]
  • 9
  • [ 867130-58-3 ]
  • [ 1242458-08-7 ]
  • [ 1242453-94-6 ]
YieldReaction ConditionsOperation in experiment
Example 16-oxo-5,6-dihydro-pyridazine-4-carboxylic acid-(1-[5-(4-fluoro-2-trifluoromethyl-phenylamino)-pyridin-2-ylmethyl]-carbamoyl}-cyclopropyl)-amide Prepared from intermediate C2 and <strong>[867130-58-3]6-oxo-1,6-dihydro-pyridazine-4-carboxylic acid</strong> according to AAV1. AAV 1: Amide CouplingA solution of the carboxylic acid component (1 mol-equivalent), triethylamine (2.5 mol-equivalents) and TBTU (1.1 mol-equivalents) in THF was stirred for 30 minutes at ambient temperature. Then the amine component (1.1 mol-equivalent as hydrochloride) was added and stirring was continued overnight. Then the mixture was evaporated down, mixed with water, made alkaline with dilute potassium carbonate solution and extracted with ethyl acetate. The product was isolated and purified by column chromatography (either silica gel or reversed phase chromatography).
  • 10
  • [ 867130-58-3 ]
  • [ 1242456-51-4 ]
  • 11
  • [ 867130-58-3 ]
  • [ 1360430-75-6 ]
  • 12
  • [ 867130-58-3 ]
  • [ 1037301-09-9 ]
  • [ 1360429-41-9 ]
YieldReaction ConditionsOperation in experiment
90% A solution of <strong>[867130-58-3]6-oxo-1,6-dihydro-pyridazine-4-carboxylic acid</strong> (10.5 g, 74.9 mmol), TBTU (25.3 g, 78.7 mmol), triethylamine (20.9 mL) and 40 mL DMF in 200 mL THF was stirred for 30 minutes at ambient temperature. Then n-butyl(S)-3-amino-tetrahydrofuran-3-carboxylate (14.0 g, 74.9 mmol) was added and the mixture was stirred further overnight. For working up the mixture was evaporated to dryness in vacuo and the residue was stirred with 200 mL ethyl acetate. This solution was washed twice with 5% sodium hydrogen carbonate solution, then dried and evaporated down. The product was thus obtained in a yield of 90% of theory. C14H19N3O5 (309.3) Thin layer chromatograph (silica gel; dichloromethane/ethanol 19:1): Rf=0.16
90% With O-(benzotriazol-1-yl)-N,N,N',N'-tetramethyluronium tetrafluoroborate; triethylamine; N,N-dimethyl-formamide; In tetrahydrofuran; at 20℃; [0373] A solution of <strong>[867130-58-3]6-oxo-1,6-dihydro-pyridazine-4-carboxylic acid</strong> (11.5 g), TBTU (25.3 g), triethylamine (20.9 mL) and 40 mL DMF in 200 mL THF was stirred for 30 minutes at ambient temperature. Then n-butyl (S)-3-amino-tetrahydrofuran-3-carboxylate (14.0 g) was added and the mixture was stirred further overnight. For working up the mixture was evaporated to dryness in vacuo and the residue was stirred with 200 mL of ethyl acetate. This solution was washed twice with 5% sodium hydrogen carbonate solution, then dried and evaporated down. The product was thus obtained in a yield of 90% of theory. [0374] C14H19N3O5 (309.3) [0375] Thin layer chromatogram (silica gel; dichloromethane/ethanol 19:1): Rf=0.16
  • 13
  • [ 867130-58-3 ]
  • (S)-6-oxo-1,6-dihydropyridazine-4-carboxylic acid (3-[5-(4-chloro-2-(trifluoromethyl)phenylamino)-3-fluoropyridin-2-ylmethyl]carbamoyl}tetrahydrofuran-3-yl)amide [ No CAS ]
  • 14
  • [ 867130-58-3 ]
  • copper(II) nitrate trihydrate [ No CAS ]
  • [ 7732-18-5 ]
  • [Cu(6-oxo-1,6-dihydropyridazine-4-carboxylic acid(-H))2(H2O)2]*3H2O [ No CAS ]
Recommend Products
Same Skeleton Products

Technical Information

Historical Records
; ;