反应 #1350593

反应方程式

3-amino-2-methylbenzoic acid

methyl isothiocyanate

bromine

→

2-Methylamino-4-methylbenzothiazole-5-carboxylic Acid

溶剂

acetic acid

acetic acid

acetic acid

反应条件

后处理

1. 1
   温度to cool
2. 2
   过滤The precipitate was filtered off
3. 3
   浓缩the filtrate was concentrated to about 50 ml
4. 4
   workup.ADDITIONthe remaining filtrate and the precipitate were added to water
5. 5
   过滤the precipitate was filtered off at 8° C
6. 6
   洗涤It was subsequently washed with water
7. 7
   其他dried

实验过程

99 g of 3-amino-2-methylbenzoic acid (0.655 mol) were initially charged in 500 ml of acetic acid and, at 80° C,. admixed with 51 g of methyl isothiocyanate (7 mol) in 100 ml of acetic acid. After 2 h, 106 g of bromine (0.66 mol) in 20 ml of acetic acid were added dropwise at 50° C. The mixture was subsequently heated at about 100° C. for 2 h and, after the reaction had ended, allowed to cool. The precipitate was filtered off, the filtrate was concentrated to about 50 ml and the remaining filtrate and the precipitate were added to water. The aqueous phase was adjusted to pH 5 and the precipitate was filtered off at 8° C. It was subsequently washed with water and dried. Yield: 66 g (42%).

来源