Triethylamine → HCID 19850149、化合物

HRID 1608005ノート

反応式

HRID 1608005 の反応式
[CH3:1][S:2](Cl)(=[O:4])=[O:3].[NH2:6][C:7]1[CH:8]=[C:9]([CH2:15][CH2:16][NH:17][C:18](=[O:23])[C:19]([F:22])([F:21])[F:20])[CH:10]=[CH:11][C:12]=1[O:13][CH3:14].C(N(CC)CC)C>ClCCl>[F:20][C:19]([F:21])([F:22])[C:18]([NH:17][CH2:16][CH2:15][C:9]1[CH:10]=[CH:11][C:12]([O:13][CH3:14])=[C:7]([NH:6][S:2]([CH3:1])(=[O:4])=[O:3])[CH:8]=1)=[O:23]

参加物

5

反応物 3

HCID 8471TriethylamineHCID 31297Methanesulfonyl chlorideHCID 12807541N-[2-(3-Amino-4-methoxyphenyl)ethyl]-2,2,2-trifluoroacetamide

生成物 1

HCID 19850149HCID 19850149、化合物収率 93.4%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

実験手順

Methanesulphonyl chloride (5.75 g, 0.05 moles) in dry dichloromethane (-50 ml) was added dropwise with stirring to N-[2-(3-amino-4-methoxyphenyl)ethyl]-2,2,2-trifluoro acetamide (13.1 g, 0.05 moles) and triethylamine (10.1 g, 7.5 ml, 0.1 mole) in dry dichloromethane (250 ml). Stirring was continued at 20° for 18 hr and the solution was then washed with dilute hydrochloric acid, saturated sodium bicarbonate solution and water, dried and evaporated. The residue on recrystallisation from benzene gave the sub-title compound (15.9 g) as ivory-coloured plates mp 129°-130°.

後処理

  1. washthe solution was then washed with dilute hydrochloric acid, saturated sodium bicarbonate solution and water
  2. customdried
  3. customevaporated
  4. customThe residue on recrystallisation from benzene

出典と根拠

ORDレコード
ord-917ab8c5fbb2477da7c69d27258382b2
出典データセット
uspto-grants-1989_09
特許番号
US04868306

反応ノート

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