反応 #4537

反応方程式

pyridinium chlorochromate

3-hydroxymethyl-5-dichloromethyl-2-phthalimidopyrazine

→

colorless crystals

収率 78.0%

3-formyl-5-dichloromethyl-2-phthalimidopyrazine

収率 78.0%

溶媒

dichloromethane

反応条件

後処理

1. 1
   ろ過filtered over silica gel
2. 2
   その他the filtrate was evaporated down

実験手順

5.1 g of pyridinium chlorochromate were added a little at a time to a solution of 4 g of 3-hydroxymethyl-5-dichloromethyl-2-phthalimidopyrazine in 80 ml of dichloromethane at 35° C., after which the mixture was stirred for 40 minutes and filtered over silica gel, and the filtrate was evaporated down. 3.1 g (76%) of colorless crystals of 3-formyl-5-dichloromethyl-2-phthalimidopyrazine of melting point 145°-146° C. (from ethyl acetate) were obtained. 1H-NMR (270 MHz, CDCl3): δ6.9 (s, 1H), 8.0 (m, 4H), 9.3 (s, 1H), 10.1 (s, 1H).

出典