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

HRID 653062

반응식

HRID 653062 반응식
[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

참가 물질

5

반응물 2

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

생성물 1

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

시약·촉매·용매 2

HCID 142844-(Dimethylamino)pyridine촉매HCID 1049Pyridine용매

반응 조건

온도
25 °C

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-9d849a59ec7c421cba41c69e61a65a96
출처 데이터셋
uspto-grants-1987_06
특허 번호
US04675331

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