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

HRID 1256942ノート

反応式

HRID 1256942 の反応式
[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

参加物

6

反応物 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

生成物 1

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

試薬・触媒・溶媒 2

HCID 6342Acetonitrile溶媒HCID 81531Diisopropylethylamine溶媒

実験手順

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).

後処理

  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%)

出典と根拠

ORDレコード
ord-7740787c91a0493ab5296f4bbfac262a
出典データセット
uspto-grants-2013_06
特許番号
US08461329B2

反応ノート

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