反应 #355732
ord-0a0551b5bf3049c0a58006b54583054c
反应方程式
2-chloromethyl-4-nitrophenol
methanol
sodium methoxide
→
expected product
2-methoxymethyl-4-nitrophenol
溶剂
反应条件
详细条件
See reaction.notes.procedure_details.
后处理
- 1温度refluxed for 2 hours 30 minutes
- 2温度the mixture was refluxed for another 30 minutes
- 3温度The resulting mixture was cooled in an ice bath
- 4其他the insoluble matter formed
- 5过滤was filtered off
- 6过滤The crystalline product was filtered off by suction
- 7干燥dried over P2O5 at 40° C
- 8其他11.4 g of crude products were isolated
- 9其他recrystallized from 15 ml of isopropyl acetate
实验过程
18.7 g (0.1 mol) of 2-chloromethyl-4-nitrophenol and 50 ml of pure methanol were mixed together and refluxed for 2 hours 30 minutes. 37 ml of sodium methoxide (0.2 mol, 5.4 N solution in MeOH) were added and the mixture was refluxed for another 30 minutes. The resulting mixture was cooled in an ice bath and diluted with 350 ml of water, and the insoluble matter formed was filtered off. The filtrate was acidified with acetic acid (10 ml). The crystalline product was filtered off by suction, reslurried in ice-cold water and then dried over P2O5 at 40° C. 11.4 g of crude products were isolated and then recrystallized from 15 ml of isopropyl acetate to give 7.5 g of expected product.