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[ CAS No. 77385-90-1 ] {[proInfo.proName]}

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Chemical Structure| 77385-90-1
Chemical Structure| 77385-90-1
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Product Details of [ 77385-90-1 ]

CAS No. :77385-90-1 MDL No. :MFCD00796343
Formula : C18H21NO2 Boiling Point : No data available
Linear Structure Formula :(C6H5CH2)2NCH2CO2C2H5 InChI Key :AFMDCFOWHWNQBP-UHFFFAOYSA-N
M.W : 283.37 Pubchem ID :3553452
Synonyms :
Chemical Name :Ethyl 2-(dibenzylamino)acetate

Safety of [ 77385-90-1 ]

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

Application In Synthesis of [ 77385-90-1 ]

* 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 [ 77385-90-1 ]

[ 77385-90-1 ] Synthesis Path-Downstream   1~2

  • 1
  • [ 77385-90-1 ]
  • [ 925-90-6 ]
  • [ 428855-17-8 ]
YieldReaction ConditionsOperation in experiment
84.3% With titanium(IV) isopropylate; In tetrahydrofuran; at 10℃;Inert atmosphere; Under an atmosphere of nitrogen, 2- (dibenzylamino) acetate (IV-1) (2.0 g, 7.0 mmol) was dissolved in tetrahydrofuran (10 ml)Tetraisopropyl titanate (0.5 g, 1.7 mmol) was added,A solution of 1M ethylmagnesium bromide in tetrahydrofuran (21 ml, 21.0 mmol) was added at 10 C,Plus,Continue stirring.TLC monitoring reaction end,Saturated ammonium chloride solution quenched,Solid precipitation.filter,The filter cake was washed with ethyl acetate (50 ml x 2)The combined organic layers were washed with saturated sodium bicarbonate solution (50 ml)The organic layer was dried over anhydrous sodium sulfate,filter,Concentrated crude,Purification by flash column chromatography (petroleum ether: ethyl acetate = 5: 1)Get the oil,A total of 1.59g,The yield was 84.3%.
60% Step 2: Preparation of 1-((diphenylmethylamino)methyl)cyclopropan-1-ol Titanium isopropoxide (622 mg, 2.33 mmol) was added to a solution of ethyl N-(phenylmethylene)glycinate (3.0 g, 11 mmol) in diethyl ether (100 mL) at room temperature. Ethylmagnesium bromide (3.0 M Et2O solution, 10.6 mL, 31.8 mmol) was added dropwise and slowly, and the mixture was stirred for 12 hours at room temperature. After the reaction was cooled to 0C, hydrochloric acid (2M, 10mL) was added slowly, then the reaction was warmed up to room temperature slowly and stirred for 30 minutes. After addition of saturated NaHCO3 aqueous solution (60 mL), the reaction solution was stirred for 10 minutes, extracted twice with CH2Cl2, and concentrated. The resulting residue was subjected to column chromatography to obtain the title compound 1-((diphenylmethylamino)methyl)cyclopropan-1-ol (1.7 g, 60%). MS m/z (ESI): 268.2 [M+H]+.
2.05 g In tetrahydrofuran; at 0 - 35℃; for 16h;Inert atmosphere; Under a nitrogen atmosphere, a 3.0 M solution of ethylmagnesium bromide in THF (9.41 mL) was added dropwise to a solution of ethyl 2-(dibenzylamino)acetate (4.0 g) and tetraisopropyl titanate (827 μL) in THF (50 mL) at 0 C., and the mixture was stirred at room temperature for 16 hr. To the reaction mixture was added saturated aqueous ammonium chloride solution, and the mixture was extracted with ethyl acetate. The extract was washed with water and saturated brine, and dried over anhydrous magnesium sulfate. The solvent was evaporated under reduced pressure, and the residue was purified by silica gel column chromatography (ethyl acetate/hexane) to give the title compound (2.05 g) as a pale-yellow oil. (0864) 1H NMR (400 MHz, DMSO-d6) δ 0.26-0.38 (2H, m), 0.49-0.60 (2H, m), 2.53 (2H, s), 3.67 (4H, s), 5.01 (1H, s), 7.17-7.25 (2H, m), 7.31 (4H, t, J=7.5 Hz), 7.35-7.46 (4H, m).
6.59 g With titanium(IV) isopropylate; In tetrahydrofuran; diethyl ether; at 0 - 35℃;Inert atmosphere; (A) 1-((Dibenzylamino)methyl)cyclopropanol To a mixture of ethyl 2-(dibenzylamino)acetate (11.2 g), titanium tetraisopropoxide (2.398 mL) and THF (130 mL), a 3 M solution of ethyl magnesium bromide in diethyl ether (26.4 mL) was added dropwise at 0 C., and the resulting mixture was stirred overnight under nitrogen atmosphere at room temperature. Saturated aqueous ammonium chloride solution was added to the reaction mixture, and the aqueous layer was extracted with ethyl acetate. The extract was washed with water and brine and then dried over anhydrous magnesium sulfate, and the solvent was distilled off under reduced pressure. The residue was purified by silica gel column chromatography (ethyl acetate/hexane) to obtain the title compound (6.59 g). 1H NMR (300 MHz, DMSO-d6) δ 0.19-0.39 (2H, m), 0.46-0.63 (2H, m), 2.53 (2H, s), 3.66 (4H, s), 5.04 (1H, s), 7.16-7.26 (2H, m), 7.27-7.35 (4H, m), 7.36-7.43 (4H, m).
With titanium(IV) isopropylate; In diethyl ether; at 0 - 20℃; for 24h; Ethyl dibenzyl glycinate (1 g, 3.5 mmol, 1.0 equiv) was dissolved in diethyl ether (10 mL) and cooled to 0 C. Ti(OiPr)4 (0.25 g, 0.88 mmol, 0.25 equiv) and EtMgBr (3.0 M in diethyl ether) (4.7 mL, 14.1 mmol, 4.0 equiv) were added, and the reaction mixture was stirred at RT for 24 h. The reaction mixture was cooled to 0 C., quenched with saturated aqueous ammonium chloride solution and extracted with EtOAc. The organic layer was washed with brine, dried over sodium sulfate, and concentrated to afford a crude residue. The crude residue was purified by silica gel column chromatography (5% EtOAc/hexane) to afford I-58A. LCMS (m/z): 268.3 [M+H]. 1H NMR (400 MHz, DMSO-d6) δ 7.39 (d, J=7.0 Hz, 4H), 7.32 (t, J=7.5 Hz, 4H), 7.23 (t, J=7.2 Hz, 2H), 5.06 (s, 1H), 3.64 (d, J=20.7 Hz, 4H), 2.53 (s, 2H), 0.57-0.54 (m, 2H), 0.33 (dd, J=6.7, 4.6 Hz, 2H).

  • 2
  • [ 77385-90-1 ]
  • [ 428855-17-8 ]
YieldReaction ConditionsOperation in experiment
6.59 g With titanium(IV) isopropylate; methylmagnesium bromide; In tetrahydrofuran; diethyl ether; at 0 - 20℃;Inert atmosphere; At 0 C.To a solution of ethyl 2- (dibenzylamino) acetate (11.2 g)Titanium tetraisopropoxide (2.398 mL) and THF (130 mL)The mixture is added dropwiseEthyl magnesium bromide in diethyl etherSolution (26.4 mL),The resulting mixture was stirred in a nitrogen atmosphere,Stir at room temperature overnight.A saturated aqueous solution of ammonium chloride was added to the reaction mixture,And the aqueous layer was extracted with ethyl acetate.The extract was washed with water and brine, dried over anhydrous magnesium sulfate, and the solvent was removed by distillation under reduced pressure.The residue was purified by silica gel column chromatography (ethyl acetate / hexane) to give the title compound (6.59 g).
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