Triethylamine → HCID 19850149、化合物

HRID 414383ノート

反応式

HRID 414383 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-89f50f5879fb4da5b0830aafae1f45bb
出典データセット
uspto-grants-1988_12
特許番号
US04791216

反応ノート

読み込み中…