Pyridine → HCID 178500684、化合物

HRID 1713796ノート

反応式

HRID 1713796 の反応式
Cl[C:2](=[O:7])[C:3]([O:5][CH3:6])=[O:4].[NH2:8][C:9]1[CH:14]=[CH:13][C:12]([C@H:15]2[CH2:20][CH2:19][C@H:18]([CH2:21][C:22]([O:24][CH3:25])=[O:23])[CH2:17][CH2:16]2)=[CH:11][CH:10]=1.N1C=CC=CC=1>C(Cl)Cl>[CH3:25][O:24][C:22](=[O:23])[CH2:21][C@H:18]1[CH2:17][CH2:16][C@H:15]([C:12]2[CH:11]=[CH:10][C:9]([NH:8][C:2](=[O:7])[C:3]([O:5][CH3:6])=[O:4])=[CH:14][CH:13]=2)[CH2:20][CH2:19]1

参加物

5

反応物 3

HCID 1049PyridineHCID 79846Methyl chloroglyoxylateHCID 178500653HCID 178500653、化合物

生成物 1

HCID 178500684HCID 178500684、化合物

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

実験手順

Methyl chloro(oxo)acetate (0.842 mL) was added to a stirred solution of methyl [trans-4-(4-aminophenyl)cyclohexyl]acetate (1740 mg) and pyridine (0.689 mL) in DCM (50 mL) at 0° C. After the addition was complete the mixture was allowed to warm to ambient temperature and stirred for 64 hours. The solution was diluted with DCM (100 mL), washed with water (50 mL) and brine (50 mL), then dried and concentrated in vacuo to give the title compound (2267 mg) as a solid; 1H NMR δ 7.60 (2H, d), 7.18 (2H, d), 3.83 (3H, s), 3.58 (3H, s), 2.58-35 (1H+DMSO, m), 2.21 (2H, d), 1.75 (5H, m), 1.43 (2H, m), 1.12 (2H, m); MS m/e MH− 332.

後処理

  1. additionAfter the addition
  2. washwashed with water (50 mL) and brine (50 mL)
  3. customdried
  4. concentrationconcentrated in vacuo

出典と根拠

ORDレコード
ord-1889c2b9165441779f181ab59cfd58a7
出典データセット
uspto-grants-2010_09
特許番号
US07795283B2

反応ノート

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