反应 #1350589

ord-1457830cd9ea443bbca17272e72d3e21

反应方程式

COC(=O)c1cccc(NC(N)=S)c1C
N-(2-methyl-3-methoxycarbonylphenyl)thiourea
BrBr
bromine
COC(=O)c1ccc2sc(N)nc2c1C
Methyl 2-Amino-4-methylbenzothiazole-5-carboxylate

反应条件

温度
0°CELSIUS
详细条件
See reaction.notes.procedure_details.

后处理

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

实验过程

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%).

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US06541423B1uspto-grants-2003_04