Ethanol → HCID 67444892, 화합물

HRID 1371887노트

반응식

HRID 1371887 반응식
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

참가 물질

5

반응물 3

HCID 702EthanolHCID 6367Acetyl chlorideHCID 21071661HCID 21071661, 화합물

생성물 1

HCID 67444892HCID 67444892, 화합물

시약·촉매·용매 1

HCID 3283Diethyl Ether용매

실험 절차

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.

후처리

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

출처 및 근거

ORD 기록
ord-2b55b7cfdf124b03b2e64663f586563a
출처 데이터셋
uspto-grants-2007_01
특허 번호
US07157488B2

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