反応 #60578

反応方程式

ethyl 3-oxo-3-(4-pyridyl)propionate

N-methyl thiourea

1,8-diazabicyclo[5,4,0]-7-undecene

methanesulfonic acid

→

title compound

収率 72.1%

2-mercapto-3-methyl-6-pyridin-4-yl-3H-pyrimidin-4-one

収率 72.1%

溶媒

water

反応条件

後処理

1. 1
   洗浄The precipitate was washed with water
2. 2
   ろ過filtered
3. 3
   その他dried

実験手順

A solution of ethyl 3-oxo-3-(4-pyridyl)propionate (29.0 g, 150 mmol), N-methyl thiourea (40.6 g, 450 mmol) and 1,8-diazabicyclo[5,4,0]-7-undecene (22.4 ml, 150 mmol) was refluxed for 4 hours and the solution of methanesulfonic acid (14.4 g, 150 mmol) in water (50 ml) was added after cooling by ice-water. The precipitate was washed with water, filtered and dried to give the title compound (23.7 g, 72%).

出典