HRID24289

反应详情

EQUATION

反应方程式

HRID 24289 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
70 °C

PROCEDURE

实验过程

A 5-necked flask equipped with mechanical overhead stirrer, gas inlet tube, reflux condenser and a thermometer was charged with 4-nitrophenol (100 g, 0.72 mol). Concentrated HCl 932%, 1.3 L), conc. H2SO4 (98%, 10 mL) and formaldehyde dimethylacetal (152.4 g, 2 moles) were added and the mixture was heated to 70° C. Gaseous HCl was bubbled through the mixture for 4 hours. During this time a thick white precipitate formed. The suspension was cooled to 0° C., the precipitate was isolated by vacuum filtration and the yellow powder was dried over night under vacuum to give 108.76 g of slightly impure 2-chloromethyl-4-nitrophenol (about 76% yield).

WORKUP

后处理

  1. customA 5-necked flask equipped with mechanical overhead stirrer, gas inlet tube
  2. temperaturereflux condenser
  3. customGaseous HCl was bubbled through the mixture for 4 hours
  4. customDuring this time a thick white precipitate formed
  5. temperatureThe suspension was cooled to 0° C.
  6. customthe precipitate was isolated by vacuum filtration
  7. customthe yellow powder was dried over night under vacuum