Water → HCID 19850164, 화합물

HRID 1608008노트

반응식

HRID 1608008 반응식
[NH2:1][C:2]1[CH:3]=[C:4]([CH2:10][CH2:11][NH:12][C:13](=[O:18])[C:14]([F:17])([F:16])[F:15])[CH:5]=[CH:6][C:7]=1[O:8][CH3:9].I[CH3:20].O>CN(C)C=O>[F:17][C:14]([F:15])([F:16])[C:13]([NH:12][CH2:11][CH2:10][C:4]1[CH:5]=[CH:6][C:7]([O:8][CH3:9])=[C:2]([NH:1][CH3:20])[CH:3]=1)=[O:18]

참가 물질

5

반응물 3

HCID 962WaterHCID 6328Methyl iodideHCID 12807541N-[2-(3-Amino-4-methoxyphenyl)ethyl]-2,2,2-trifluoroacetamide

생성물 1

HCID 19850164HCID 19850164, 화합물수율 11%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

N-[2-(3-Amino-4-methoxyphenyl)ethyl]-2,2,2-trifluoro acetamide (26.2 g., 0.2 mole) and iodomethane (14.0 g., 6.2 ml., 0.2 mole) in dry dimethylformamide (500 ml) were stirred under nitrogen for 3 hr. The solution was poured into water and the suspension extracted with ethyl acetate. Evaporation of the extracts afforded an oil which was separated by high pressure liquid chromatography on silica using 1% methanol in dichloromethane as eluant. Evaporation of the fractions containing the major bond afforded the sub-title compound (6.1 g) as a white solid mp 65°-67°. The hydrochloride, prepared in the usual way, had mp 153°-155°.

후처리

  1. extractionthe suspension extracted with ethyl acetate
  2. customEvaporation of the extracts
  3. customafforded an oil which
  4. customwas separated by high pressure liquid chromatography on silica using 1% methanol in dichloromethane as eluant
  5. customEvaporation of the fractions
  6. additioncontaining the major bond

출처 및 근거

ORD 기록
ord-bbfd73b82c5d4fe4ac88aeccc6ca3a2c
출처 데이터셋
uspto-grants-1989_09
특허 번호
US04868306

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