2-Amino-6-(trifluoromethyl)benzothiazole → N-(6-trifluoromethylbenzothiazol-2-yl)-2-chloro-6-fluorobenzamide

HRID 653062ノート

反応式

HRID 653062 の反応式
[Cl:1][C:2]1[CH:10]=[CH:9][CH:8]=[C:7]([F:11])[C:3]=1[C:4](Cl)=[O:5].[NH2:12][C:13]1[S:14][C:15]2[CH:21]=[C:20]([C:22]([F:25])([F:24])[F:23])[CH:19]=[CH:18][C:16]=2[N:17]=1>CN(C)C1C=CN=CC=1.N1C=CC=CC=1>[F:25][C:22]([F:23])([F:24])[C:20]1[CH:19]=[CH:18][C:16]2[N:17]=[C:13]([NH:12][C:4](=[O:5])[C:3]3[C:7]([F:11])=[CH:8][CH:9]=[CH:10][C:2]=3[Cl:1])[S:14][C:15]=2[CH:21]=1

参加物

5

反応物 2

HCID 27359552-Amino-6-(trifluoromethyl)benzothiazoleHCID 27365472-Chloro-6-fluorobenzoyl chloride

生成物 1

HCID 13798347N-(6-trifluoromethylbenzothiazol-2-yl)-2-chloro-6-fluorobenzamide収率 66.8%

試薬・触媒・溶媒 2

HCID 142844-(Dimethylamino)pyridine触媒HCID 1049Pyridine溶媒

反応条件

温度
25 °C

実験手順

At 0 to 5° C., 2-chloro-6-fluorobenzoyl chloride (1.93 g) was added dropwise to a solution composed of 2-amino-6-trifluoromethylbenzothiazole (2.18 g), pyridine (30 ml) and 4-dimethylaminopyridine (0.1 g). The reaction mixture was stirred at room temperature (20 to 30° C.) for one day, and then the pyridine was evaporated. Water was added to the residue, and the mixture was stirred. The resulting crystals were collected by filtration, and thoroughly washed with water. Recrystallization from ethanol gave the desired N-(6-trifluoromethylbenzothiazol-2-yl)-2-chloro-6-fluorobenzamide (2.5 g).

後処理

  1. customthe pyridine was evaporated
  2. additionWater was added to the residue
  3. stirringthe mixture was stirred
  4. filtrationThe resulting crystals were collected by filtration
  5. washthoroughly washed with water
  6. customRecrystallization from ethanol

出典と根拠

ORDレコード
ord-9d849a59ec7c421cba41c69e61a65a96
出典データセット
uspto-grants-1987_06
特許番号
US04675331

反応ノート

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