Triethylamine → 4-bromo-N-(4-bromo-2-fluorobenzyl)-2-nitrobenzamide

HRID 569809

反応式

HRID 569809 の反応式
[Br:1][C:2]1[CH:9]=[CH:8][C:5]([CH2:6][NH2:7])=[C:4]([F:10])[CH:3]=1.C(N(CC)CC)C.[Br:18][C:19]1[CH:27]=[CH:26][C:22]([C:23](Cl)=[O:24])=[C:21]([N+:28]([O-:30])=[O:29])[CH:20]=1>C(Cl)(Cl)Cl>[Br:18][C:19]1[CH:27]=[CH:26][C:22]([C:23]([NH:7][CH2:6][C:5]2[CH:8]=[CH:9][C:2]([Br:1])=[CH:3][C:4]=2[F:10])=[O:24])=[C:21]([N+:28]([O-:30])=[O:29])[CH:20]=1

参加物

5

反応物 3

HCID 8471TriethylamineHCID 3770848(4-Bromo-2-fluorophenyl)methanamineHCID 189198804-Bromo-2-nitrobenzoyl chloride

生成物 1

HCID 144589874-bromo-N-(4-bromo-2-fluorobenzyl)-2-nitrobenzamide収率 81.9%

試薬・触媒・溶媒 1

HCID 6212Chloroform溶媒2 回

実験手順

To a solution of 4-bromo-2-fluorobenzylamine (2.3 g) and triethylamine (1.55 ml) in chloroform (40 ml) was added dropwise a solution of 4-bromo-2-nitrobenzoyl chloride (2.69 g) in chloroform (10 ml) at 0° C. with stirring and the mixture was stirred at the same temperature for 1 hour. The reaction mixture was washed in turn with diluted aqueous hydrochloric acid and water, and then dried. Evaporation of the solvent followed by recrystallization from diethyl ether gave 4-bromo-N-(4-bromo-2-fluorobenzyl)-2-nitrobenzamide (3.60 g).

後処理

  1. stirringthe mixture was stirred at the same temperature for 1 hour
  2. washThe reaction mixture was washed in turn with diluted aqueous hydrochloric acid and water
  3. customdried
  4. customEvaporation of the solvent
  5. customfollowed by recrystallization from diethyl ether

出典と根拠

ORDレコード
ord-83fb32c6a6f5421bb4ce4068b5c5dfb5
出典データセット
uspto-grants-1988_03
特許番号
US04734419

関連ノート

読み込み中…