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[ CAS No. 3230-65-7 ] {[proInfo.proName]}

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Chemical Structure| 3230-65-7
Chemical Structure| 3230-65-7
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Product Details of [ 3230-65-7 ]

CAS No. :3230-65-7 MDL No. :MFCD00033714
Formula : C9H9N Boiling Point : -
Linear Structure Formula :- InChI Key :NKSZCPBUWGZONP-UHFFFAOYSA-N
M.W : 131.17 Pubchem ID :76705
Synonyms :

Safety of [ 3230-65-7 ]

Signal Word:Danger Class:6.1
Precautionary Statements:P262-P264-P270-P280-P301+P312+P330-P302+P352+P310-P305+P351+P338-P332+P313-P337+P313-P361+P364-P405-P501 UN#:2811
Hazard Statements:H302-H310-H315-H319 Packing Group:Ⅱ
GHS Pictogram:

Application In Synthesis of [ 3230-65-7 ]

* 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 [ 3230-65-7 ]

[ 3230-65-7 ] Synthesis Path-Downstream   1~7

  • 1
  • [ 3230-65-7 ]
  • [ 925-90-6 ]
  • [ 25939-81-5 ]
  • 2
  • [ 23069-99-0 ]
  • [ 3230-65-7 ]
YieldReaction ConditionsOperation in experiment
95% With PPA; phosphorus pentoxide; at 170℃; for 18h; Example 1: Preparation of 3,4-dihydroisoquinoline (1, R1, R3, R3', R4, R4', R5, R6, R7, R8=H) To a flame dried 1000 ml three neck round bottomed flask, equipped with an addition funnel, dry argon inlet, magnetic stir bar, thermometer, Dean Stark trap, and heating bath is added 2- phenethylamine (8, R3, R3, R4, R4s, R5, R6, R7, R8=H) (121 gm. , 1.0 mol) and toluene (250 ml). To the addition funnel is added formic acid (46 gm. , 1 mol). The formic acid is added slowly to the stirring reaction solution over 60 minutes and solids form. Once addition is complete the reaction is brought to reflux and water removed via a Dean Stark trap. Once the reaction is complete, the toluene is removed and the product (9, Rl, R3, R3, R4, R4, R5, R6, R7, R8=H) is purified by vacuum distillation. Formamide (9, Rl, R3, R3, R4, R4, R5, R6, R7, R8=H) is then contacted with polyphosphoric acid (747 gm) /phosphorous pentoxide (150 gm), using standard Bischler/Napieralski conditions, at 170C for 18 hours. The reaction is then neutralized with aqueous NaOH, keeping the temperature between 60-80C. Once neutral, the product is extracted with toluene to yield 3,4-dihydroisoquinoline (1, Rl, R3, Ruz R4, R4, R5, R6, R7, R8=H) in 95% yield. Product can be further purified via distillation.
85% 2) Dihydroisoquinoline; Polyphosphoric acid (4.42 kg) was heated to 80 0C under stirring and mixed with P2O5 (0.69 kg). After heating to 170 0C and stirring for 1 h at this temperature N-formyl-N-(2- phenytethyi) amin (1.32 kg, 8.84 moi) was added during 30 min. After stirring for 4 h at 170 0C the reaction was cooled down to 80 0C and carefully mixed with a 20 % solution of potassium hydroxide in water (24.75 kg) in order to result pH 7-8. The crude mixture was extracted at 60 0C with toluene (4 x 4.4 I). From the combined organic phases, which were dried over Na∑SCU, the toluene was removed under vacuum (1 mbar) at 60 0C to give dihydroisoquinone (1.0 kg, 85 % yield, 99.9 % purity via gas chromatography)
78 - 91%Chromat. With methanesulfonic acid; phosphorus pentoxide; at 115 - 160℃; for 2 - 24h;Neat (no solvent);Product distribution / selectivity; Examples 18 - 37; Also the following reaction step was varied:(10) (11) (12) with the conditions and results being listed in table 1 below:
76 - 99%Chromat. With phosphorus pentoxide; at 170 - 200℃; for 0.666667 - 1h;Neat (no solvent);Product distribution / selectivity; Examples 18 - 37; Also the following reaction step was varied:(10) (11) (12) with the conditions and results being listed in table 1 below:
56.3 g (76.1%) With PPA; In water; 1.2 Synthesis of 3,4-dihydroisoquinoline 490.0 g (5.00 mol) of polyphosphoric acid were heated to 80 C. until it could be thoroughly mixed with a metal stirrer. Then 84.0 g (0.56 mol) of <strong>[23069-99-0]N-(2-phenylethyl)formamide</strong> from stage 1 were added at 80 C. while stirring and the mixture was heated to 160 C. for 12 hours. After the reaction the mixture was poured onto 1000 ml of iced water and then stirred for 2 hours at room temperature. A pH of 12.0 was established with a 5-molar, aqueous sodium hydroxide solution. The aqueous phase was extracted with methyl tert-butyl ether. The combined organic phases were dried with magnesium sulfate and completely evaporated in a rotary evaporator, resulting in a dark brown oil. The oil was distilled under vacuum (40 mbar/115 C.) and accumulated in the form of a clear, light-brown liquid, which was used in the third stage. Yield: 56.3 g (76.1%); 1H-NMR (400 MHz, DMSO-d6): δ [ppm]=2.68 (t, 2H); 3.65 (t, 2H); 7.23 (d, 1H); 7.34 (m, 2H); 7.41 (d, 1H); 8.34 (s, 1H); 13C-NMR (400 MHz, DMSO-d6): δ [ppm]=25.4; 48.0; 127.5; 127.8; 128.9; 131.5; 137.0; 160.7.
56.3 g (76%) With PPA; In water; 1.2 Synthesis of 3,4-dihydroisoquinoline 490.0 g (5.00 mol) of polyphosphoric acid were heated to 80 C. until it could be thoroughly mixed with a metal stirrer. Then 84.0 g (0.56 mol) of <strong>[23069-99-0]N-(2-phenylethyl)formamide</strong> from stage 1 was added at 80 C. while stirring and the mixture was heated to 160 C. for 12 hours. After the reaction the mixture was poured onto 1000 ml of iced water and then stirred for 2 hours at room temperature. A pH of 12.0 was established with a 5-molar, aqueous sodium hydroxide solution. The aqueous phase was extracted with methyl t-butyl ether. The combined organic phases were dried with magnesium sulfate and completely evaporated in a rotary evaporator, resulting in dark brown oil. The oil was distilled under vacuum (40 mbar/115 C.) and accumulated in the form of a clear, light-brown liquid, which was used in the third stage. Yield: 56.3 g (76%); 1H-NMR (400 MHz, DMSO-d6): δ [ppm]=2.68 (t, 2H); 3.65 (t, 2H); 7.23 (d, 1H); 7.34 (m, 2H); 7.41 (d, 1H); 8.34 (s, 1H); 13C-NMR (400 MHz, DMSO-d6): δ [ppm]=25.4; 48.0; 127.5; 127.8; 128.9; 131.5; 137.0; 160.7.
5 g With polyphosphoric acid; at 160℃; 2-Phenylethylamine (30.0 g, 0.248 mol) and ethyl formate were heated at reflux for 2 days. Removal of excess ethyl formate under vacuum gave the <strong>[23069-99-0]N-phenethylformamide</strong> in quantitative yield (37.0 g) as a colorless oil. 1H NMR spectrum (CDCl3), δ, ppm (J, Hz): 8.10 (1H, s, CHO); 7.29 (2H, t, J = 7.2, H Ar); 7.24-7.13 (3H, m, H Ar); 6.7-6.2 (1H, br. s, NH); 3.50 (2H, t, J = 7.0, CH2); 2.81 (2H, t, J =7.0, CH2). 13C NMR spectrum (CDCl3), δ, ppm: 161.4; 138.6; 128.8; 128.7; 126.6; 39.2; 35.5. Crude 2-phenylethylamine (7.0 g, 0.47 mol) and polyphosphoric acid (20 ml) were heated at 160C overnight. The reaction mixture was cooled to room temperature and made basic with 5 M NaOH; a white precipitate formed. The precipitate was filtered off, and the filtrate was extracted three times with ethyl acetate. The combined organic layer was dried over sodium sulfate, filtered, and concentrated in vacuo to yield compound 2 (5.0 g, 81%) as a pale-yellow oil. 1H NMR spectrum (CDCl3), δ, ppm (J, Hz): 8.31 (1H, t, J = 2.3, H Ar); 7.36-7.20 (3H, m, H Ar); 7.19-7.05 (1H, m, H Ar); 3.83-3.70 (2H, m, CH2); 2.81-2.69 (2H, m, CH2). 13C NMR spectrum (CDCl3), δ, ppm: 160.7; 136.7; 131.7; 128.9; 127.8; 127.6; 127.5; 47.8; 25.4.

  • 3
  • [ 3230-65-7 ]
  • [ 7584-05-6 ]
  • [ 131250-24-3 ]
  • 4
  • [ 23069-99-0 ]
  • [ 3230-65-7 ]
  • [ 64-04-0 ]
YieldReaction ConditionsOperation in experiment
30 - 95%Chromat.; 4 - 20%Chromat. With phosphorus pentoxide; at 170 - 200℃; for 0.666667 - 2h;Neat (no solvent);Product distribution / selectivity; Examples 18 - 37; Also the following reaction step was varied:(10) (11) (12) with the conditions and results being listed in table 1 below:
36%Chromat.; 1%Chromat. With methanesulfonic acid; phosphorus pentoxide; at 170℃; for 0.666667h;Neat (no solvent);Product distribution / selectivity; Examples 18 - 37; Also the following reaction step was varied:(10) (11) (12) with the conditions and results being listed in table 1 below:
49 - 81%Chromat.; 1 - 19%Chromat. With methanesulfonic acid; phosphorus pentoxide; at 130 - 140℃; for 3 - 4h;Neat (no solvent);Product distribution / selectivity; Examples 18 - 37; Also the following reaction step was varied:(10) (11) (12) with the conditions and results being listed in table 1 below:
34%Chromat.; 18%Chromat. With phosphorus pentoxide; In 1,2-dichloro-benzene; at 170 - 180℃; for 0.666667h;Product distribution / selectivity; Examples 18 - 37; Also the following reaction step was varied:(10) (11) (12) with the conditions and results being listed in table 1 below:

  • 5
  • [ 3230-65-7 ]
  • [ 7635-54-3 ]
  • C20H28NO2(1+)*Cl(1-) [ No CAS ]
YieldReaction ConditionsOperation in experiment
In toluene; at 20℃; for 24h; General procedure for preparing diastereomeric products4 and 5: A Schlenk under a nitrogen atmosphere was charged with 3,4- dihydroisoquinoline (1.0 mmol). (-)-Menthyl chloroformate (1.0 mmol) and toluene (2 ml_) were subsequently added. The reaction mixture was stirred at room temperature over a period of 24 hours. Naphthol or a naphthol derivative <n="33"/>(1.0 mmol) was then added and the resulting mixture was stirred for another 24 hours. After being transferred to a round bottom flask comprising chloroform, the solvent was removed and the resulting diastereomers were separated by flash column chromatography on silica gel (hexane/dichloromethane = 2:1 , 1 :1 ).
  • 6
  • [ 3230-65-7 ]
  • [ 20197-92-6 ]
  • [ 133528-06-0 ]
YieldReaction ConditionsOperation in experiment
78% In N,N-dimethyl-formamide; at 95℃; for 20h;Inert atmosphere; General procedure: To a solution isotaic anhydride (usually 0.5 mmol) in anhydrous DMF (3 mL) was added 3,4-dihydroisoquinoline or 4,9-dihydro-3H-pyrido[3,4-b]indole (0.65mmol, 1.3 eq) and the reaction mixture was stirred at 95 °C for 20 hrs. To the cooled mixture were added 20 mL of water drop wise while stirring. The precipitated solid was collected by filtration, washed with water, dried in vacuo to give the target.
  • 7
  • [ 271-34-1 ]
  • [ 3230-65-7 ]
  • 3-(1,2,3,4-tetrahydroisoquinolin-1-yl)-5-azaindole [ No CAS ]
YieldReaction ConditionsOperation in experiment
72% With toluene-4-sulfonic acid; In neat (no solvent); at 100℃; for 2.5h;Microwave irradiation; the mixture of the cyclic imine 3,4-dihydroisoquinoline (66 mg, 0.50 mmol);6,7-dihydrothieno[3,2-c]pyridine (51 mg, 0.38 mmol); 3,4-dihydro--carboline (63 mg, 0.38 mmol) or4,5-dihydro-3H-benz[c]azepine (55.3 mg, 0.38 mmol); and the electron-rich aromatic compound (7-, 6-,4-, or <strong>[271-34-1]5-azaindole</strong> (30 mg, 0.25 mmol)) were placed in a 10 mL pressurized reaction vial and heated ina microwave reactor, under the conditions given in Tables 1-3. In the case of <strong>[271-34-1]5-azaindole</strong>, 10 mol % ofp-TSA (4.3 mg, 0.025 mmol) as a catalyst was also added.
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