2-(4-Chlorophenyl)ethylamine → Methyl (4-{[2-(4-chlorophenyl)ethyl]carbamoyl}phenyl)acetate

HRID 1256942노트

반응식

HRID 1256942 반응식
[CH3:1][O:2][C:3](=[O:14])[CH2:4][C:5]1[CH:13]=[CH:12][C:8]([C:9]([OH:11])=O)=[CH:7][CH:6]=1.F[P-](F)(F)(F)(F)F.N1(OC(N(C)C)=[N+](C)C)C2N=CC=CC=2N=N1.[Cl:39][C:40]1[CH:45]=[CH:44][C:43]([CH2:46][CH2:47][NH2:48])=[CH:42][CH:41]=1>C(#N)C.C(N(CC)C(C)C)(C)C>[Cl:39][C:40]1[CH:45]=[CH:44][C:43]([CH2:46][CH2:47][NH:48][C:9]([C:8]2[CH:7]=[CH:6][C:5]([CH2:4][C:3]([O:2][CH3:1])=[O:14])=[CH:13][CH:12]=2)=[O:11])=[CH:42][CH:41]=1

참가 물질

6

반응물 3

HCID 674302-(4-Chlorophenyl)ethylamineHCID 9886157Methanaminium, N-((dimethylamino)(3H-1,2,3-triazolo(4,5-b)pyridin-3-yloxy)methylene)-N-methyl-, hexafluorophosphate(1-) (1:1)HCID 138161444-(2-Methoxy-2-oxoethyl)benzoic acid

생성물 1

HCID 86659540Methyl (4-{[2-(4-chlorophenyl)ethyl]carbamoyl}phenyl)acetate

시약·촉매·용매 2

HCID 6342Acetonitrile용매HCID 81531Diisopropylethylamine용매

실험 절차

To a solution of 4-(2-methoxy-2-oxoethyl)benzoic acid (1.00 g) in acetonitrile (50 ml), N,N-diisopropyl ethyl amine (2.63 ml), O-(7-azabenzotriazol-1-yl)-1,1,3,3-tetramethyluronium hexafluorophosphate (2.94 g) and 2-(4-chlorophenyl)ethylamine (790 ml) were added, and the mixed solution was stirred at room temperature for 16 hours. The solvent was removed by evaporation under reduced pressure, and the resulting crude product was purified by column chromatography (neutral OH type silica gel, ethyl acetate/n-hexane=30 to 50%) to give methyl (4-{[2-(4-chlorophenyl)ethyl]carbamoyl}phenyl)acetate (2.02 g).

후처리

  1. customThe solvent was removed by evaporation under reduced pressure
  2. customthe resulting crude product was purified by column chromatography (neutral OH type silica gel, ethyl acetate/n-hexane=30 to 50%)

출처 및 근거

ORD 기록
ord-7740787c91a0493ab5296f4bbfac262a
출처 데이터셋
uspto-grants-2013_06
특허 번호
US08461329B2

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