反応 #1350594

ord-293ef6d524064eb3bf4c40e69bbc5979

反応方程式

ClCCCl
EDC
CNc1nc2c(C)c(C(=O)O)ccc2s1
2-methylamino-4-methylbenzothiazole-5-carboxylic acid
Cn1nccc1O
1-methyl-5-hydroxypyrazole
CC#N
acetonitrile
CNc1nc2c(C)c(C(=O)Oc3ccnn3C)ccc2s1
1-Methylpyrazol-5-yl 2-Methylamino-4-methylbenzothiazole-5-carboxylate

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    抽出the mixture was extracted with ethyl acetate
  2. 2
    洗浄The organic phase was washed
  3. 3
    その他dried
  4. 4
    その他the product was then purified by crystallization

実験手順

3.1 g of 2-methylamino-4-methylbenzothiazole-5-carboxylic acid (0.014 mol) and 1.4 g of 1-methyl-5-hydroxypyrazole (0.015 mol) were dissolved in 110 ml of abs. acetonitrile and admixed with 2.67 g of EDC (0.014 mol), 1,2 ml of triethylamine and a catalytic amount of DMAP. After the reaction had ended, the solution was poured into water and the mixture was extracted with ethyl acetate. The organic phase was washed and dried, and the product was then purified by crystallization. Yield: 2.2 g (52%).

出典

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