反応 #1350595

ord-65c5ee7c7cf14fd28ac87b0307fa786b

反応方程式

ClCCCl
EDC
Cn1nnc2cc(C(=O)O)ccc21
1-methylbenzotriazole-5-carboxylic acid
Cn1nccc1O
1-methyl-5-hydroxypyrazole
CC#N
acetonitrile
Cn1nccc1OC(=O)c1ccc2c(c1)nnn2C
1-Methylpyrazol-5-yl 1-Methylbenzotriazole-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

1.5 g of 1-methylbenzotriazole-5-carboxylic acid (8.5 mmol) and 0.87 g of 1-methyl-5-hydroxypyrazole (8.9 mmol) were dissolved in 70 ml of abs. acetonitrile and admixed with 1.62 g of EDC (8.5 mmol), 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: 0.77 g (35%).

出典

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