反応 #314765

反応方程式

material

5-amino-6-methyl-4-pyrimidinecarboxylic acid monosodium salt

methanesulfonyl chloride

methanesulfonyl chloride

3-chloro-1-(3-chloro-2-pyridinyl)-1H-pyrazol-5-carboxylic acid

3-chloro-1-(3-chloro-2-pyridinyl)-1H-pyrazole-5-carboxylic acid

triethylamine

triethylamine

→

title compound

収率 22.2%

5-[[[3-Chloro-1-(3-chloro-2-pyridinyl)-1H-pyrazol-5-yl]carbonyl]amino]-N,6-dimethyl-4-pyrimidinecarboxamide

収率 22.2%

溶媒

water

acetonitrile

acetonitrile

反応条件

後処理

1. 1
   ろ過Filtration

実験手順

To a solution of 0.26 mL (3.3 mmol) of methanesulfonyl chloride in 18 mL of acetonitrile at 0° C. was added 0.77 g (3.0 mmol) of 3-chloro-1-(3-chloro-2-pyridinyl)-1H-pyrazol-5-carboxylic acid from Step J. 0.42 mL (3.0 mmol) of triethylamine in 9 mL of acetonitrile was added dropwise. After 20 minutes at 0° C., 0.525 g (3.0 mmol) of material from Step F was added. After 15 minutes 0.42 mL (3.0 mmol) of triethylamine was added dropwise. After 2 hours 0.26 mL (3.3 mmol) of methanesulfonyl chloride was added. After stirring overnight. The reaction mixture was poured into water. Filtration afforded 0.27 g of the title compound.

出典