Ammonia → 3,4-Dichloro-5-isothiazolecarboxylic acid amide

HRID 642919노트

반응식

HRID 642919 반응식
[Cl:1][C:2]1[C:6]([Cl:7])=[C:5]([C:8](Cl)=[O:9])[S:4][N:3]=1.[NH3:11]>O>[Cl:1][C:2]1[C:6]([Cl:7])=[C:5]([C:8]([NH2:11])=[O:9])[S:4][N:3]=1

참가 물질

4

반응물 2

HCID 222Ammonia2회HCID 109768863,4-Dichloro-5-isothiazolecarbonyl chloride

생성물 1

HCID 113330673,4-Dichloro-5-isothiazolecarboxylic acid amide수율 82%

시약·촉매·용매 1

HCID 962Water용매

실험 절차

At 0 to 10° C., 50.1 g (0.2 mol) of 3,4-dichloro-isothiazole-5-carbonyl chloride are added dropwise with stirring over a period of 30 minutes to 82 g (1.2 mol) of concentrated ammonia. After the addition, another 41 g (0.6 mol) of concentrated ammonia are added and the mixture is diluted with 70 ml of water. The mixture is allowed to warm to room temperature and stirred at this temperature for 45 minutes. The resulting precipitate is filtered off with suction, washed successive with water and petroleum ether and dried. In this manner, 32.3 g (81.8% of theory) of 3,4-dichloro-isothiazole-5-carboxamide are obtained in the form of a solid of melting point 156 to 158° C.

후처리

  1. additionAfter the addition
  2. filtrationThe resulting precipitate is filtered off with suction
  3. washwashed successive with water and petroleum ether
  4. customdried

출처 및 근거

ORD 기록
ord-0d80440c6e0145608b994dc1833c5b36
출처 데이터셋
uspto-grants-2010_04
특허 번호
US07696355B2

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