反应 #1597027

反应方程式

thionyl chloride

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

thionyl chloride

methanol

thionyl chloride

→

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

反应条件

后处理

1. 1
   温度the mixture is warmed at 80° C. for a further 2 h
2. 2
   其他the reaction
3. 3
   温度the mixture is warmed at 80° C. for a further 2 h
4. 4
   其他For work-up, 1000 ml of methanol are removed in a rotary evaporator
5. 5
   过滤the resultant residue is filtered off
6. 6
   其他The mother liquor is reduced to about 200 ml in the rotary evaporator
7. 7
   其他the crystals formed
8. 8
   过滤are filtered off
9. 9
   其他dried to constant weight at 50° C. in a vacuum
10. 10
    其他drying cabinet

实验过程

78.8 g of 3-(5-hydroxypyrimidin-2-yl)benzoic acid are suspended in 1.4 l of absolute methanol, and 32.7 ml of thionyl chloride (449.8 mmol) are subsequently carefully added dropwise at RT. The reaction batch is warmed at 80° C. for 2 h. A further 20 ml of thionyl chloride (275.7 mmol) are added, and the mixture is warmed at 80° C. for a further 2 h. In order to complete the reaction, a further 10 ml of thionyl chloride (137.8 mmol) are added, and the mixture is warmed at 80° C. for a further 2 h. For work-up, 1000 ml of methanol are removed in a rotary evaporator, and the resultant residue is filtered off. The mother liquor is reduced to about 200 ml in the rotary evaporator, and the crystals formed are filtered off. The two crystal batches are combined, dried to constant weight at 50° C. in a vacuum drying cabinet.

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