Water → HCID 19850164、化合物

HRID 542540ノート

反応式

HRID 542540 の反応式
[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]

参加物

5

反応物 3

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

生成物 1

HCID 19850164HCID 19850164、化合物収率 22.1%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

N-[2-(3amino-4-methoxyphenyl]ethyl]-2,2,2-trifluoro acetamide (26.2 g., 0.1 mole) and iodomethane (14.0 g., 6.2 ml , 0.1 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°.

後処理

  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

出典と根拠

ORDレコード
ord-60bccf60e2c240ad940e0145b5c74ec8
出典データセット
uspto-grants-1987_04
特許番号
US04657929

反応ノート

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