反应 #1350591

ord-0e927be09fb34b51bea0202baafbd83b

反应方程式

ClCCCl
EDC
Cc1c(C(=O)O)ccc2c1N(Cl)CS2
3-chloro-4-methylbenzothiazol-5-carboxylic acid
Cn1nccc1O
1-methyl-5-hydroxypyrazole
CC#N
acetonitrile
Cc1c(C(=O)Oc2ccnn2C)ccc2c1N(Cl)CS2
1-Methylpyrazol-5-yl 3-Chloro-4-methylbenzothiazole-5-carboxylate

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    萃取the product was extracted with ethyl acetate
  2. 2
    洗涤The organic phase was washed
  3. 3
    其他dried
  4. 4
    其他the product was purified by crystallization/column chromatography

实验过程

1 g of 3-chloro-4-methylbenzothiazol-5-carboxylic acid (4.4 mol) and 0.46 g of 1-methyl-5-hydroxypyrazole (4.7 mol) were dissolved in 50 ml of abs. acetonitrile and admixed with 1 g of EDC, 0.7 ml of triethylamine and a catalytic amount of DMAP. After the reaction had ended, the solution was poured into water and the product was extracted with ethyl acetate. The organic phase was washed and dried and the product was purified by crystallization/column chromatography. Yield: 0.22 g (16%).

来源

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