Ethanol → HCID 67444892、化合物

HRID 1371887ノート

反応式

HRID 1371887 の反応式
C([Cl:4])(=O)C.C(O)C.[F:8][C:9]1[CH:10]=[CH:11][CH:12]=[C:13]2[C:17]=1[NH:16][CH:15]=[C:14]2[CH2:18][CH2:19][NH:20][CH2:21][C:22]1[CH:27]=[CH:26][CH:25]=[C:24]([O:28][CH2:29][C:30]([F:33])([F:32])[F:31])[CH:23]=1>C(OCC)C>[ClH:4].[F:8][C:9]1[CH:10]=[CH:11][CH:12]=[C:13]2[C:17]=1[NH:16][CH:15]=[C:14]2[CH2:18][CH2:19][NH:20][CH2:21][C:22]1[CH:27]=[CH:26][CH:25]=[C:24]([O:28][CH2:29][C:30]([F:33])([F:31])[F:32])[CH:23]=1

参加物

5

反応物 3

HCID 702EthanolHCID 6367Acetyl chlorideHCID 21071661HCID 21071661、化合物

生成物 1

HCID 67444892HCID 67444892、化合物

試薬・触媒・溶媒 1

HCID 3283Diethyl Ether溶媒

実験手順

Add dropwise acetyl chloride (2.3 mL, 32.4 mmol) to anhydrous ethanol (50 mL) and stir the solution for 10 min at ambient temperature and add to a solution N-(2-(7-fluoro-1H-indol-3-yl)ethyl)-3-(2,2,2-trifluoroethoxy)benzylamine (10.7 g, 29.2 mmol) in diethyl ether. Concentrate the resulting solution under reduced pressure to give a yellow solid. Recrystallize the yellow solid from ethyl acetate/methanol to give the title compound: mp 163–164° C.; MS(m/e): 367 (M+1), 365 (M−1); Calculated for C19H18F4N2O HCl: Calcd: C, 56.65; H, 4.75; N, 6.90. Found: C, 56.45; H, 4.54; N, 6.90.

後処理

  1. concentrationConcentrate the resulting solution under reduced pressure
  2. customto give a yellow solid
  3. customRecrystallize the yellow solid from ethyl acetate/methanol

出典と根拠

ORDレコード
ord-2b55b7cfdf124b03b2e64663f586563a
出典データセット
uspto-grants-2007_01
特許番号
US07157488B2

反応ノート

読み込み中…