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

HRID 650865ノート

反応式

HRID 650865 の反応式
[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

参加物

4

反応物 2

HCID 222Ammonia2 回HCID 109768863,4-Dichloro-5-isothiazolecarbonyl chloride

生成物 1

HCID 113330673,4-Dichloro-5-isothiazolecarboxylic acid amide収率 82%

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

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.

後処理

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

出典と根拠

ORDレコード
ord-9610882382304397a05011d9881fe56f
出典データセット
uspto-grants-2001_08
特許番号
US06277791B1

反応ノート

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