反应 #417979

反应方程式

thionyl chloride

thionyl chloride

3-(5-hydroxypyrimidin-2-yl)benzoic acid

methanol

thionyl chloride

→

methyl 3-(5-hydroxypyrimidin-2-yl)benzoate

反应条件

后处理

1. 1
   workup.ADDITIONAfter each addition
2. 2
   其他The reaction mixture is evaporated to a volume of about 300 ml in vacuo
3. 3
   其他The precipitate formed
4. 4
   过滤is filtered off
5. 5
   其他dried in vacuo
6. 6
   其他=2.58 min (method A)

实验过程

32.7 ml (445 mmol) of thionyl chloride are added to a suspension of 88.0 g (366 mmol) of 3-(5-hydroxypyrimidin-2-yl)benzoic acid in 1.4 l of methanol, and the mixture is heated at 80° C. for 2 hours. 20 ml (276 mmol) of thionyl chloride and, after 2 hours, a further 10 ml (138 mmol) of thionyl chloride are then added. After each addition, the reaction mixture is stirred at 80° C. for 2 hours. The reaction mixture is evaporated to a volume of about 300 ml in vacuo. The precipitate formed is filtered off and dried in vacuo: methyl 3-(5-hydroxypyrimidin-2-yl)benzoate as brownish crystals; m.p. 219-223°; ESI 231 (M+H); HPLC: Rt.=2.58 min (method A).

来源