反応 #1350589

反応方程式

N-(2-methyl-3-methoxycarbonylphenyl)thiourea

bromine

→

Methyl 2-Amino-4-methylbenzothiazole-5-carboxylate

溶媒

chlorobenzene

chlorobenzene

反応条件

後処理

1. 1
   温度The reaction mixture was heated at 90° C. for 3 h
2. 2
   ろ過the precipitate was filtered off with suction
3. 3
   洗浄washed with methylene chloride
4. 4
   workup.DISSOLUTIONThe precipitate was then dissolved in ethyl acetate
5. 5
   抽出extracted with sodium bicarbonate solution
6. 6
   洗浄After washing
7. 7
   その他drying
8. 8
   その他the product was obtained

実験手順

56 g of N-(2-methyl-3-methoxycarbonylphenyl)thiourea (0.25 mol) were dissolved in 2 l of chlorobenzene, and the mixture was cooled to 0° C. 40 g of bromine (0.25 mol) in 100 ml of chlorobenzene were then added dropwise. The reaction mixture was heated at 90° C. for 3 h, and the precipitate was filtered off with suction and washed with methylene chloride. The precipitate was then dissolved in ethyl acetate and extracted with sodium bicarbonate solution. After washing and drying, the product was obtained by stripping off the solvent. Yield: 43 g (80%).

出典