HRID571577

反应详情

EQUATION

反应方程式

HRID 571577 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

856 g of 2-nitrobenzenesulfonyl chloride and 7 L of methanol are placed in a reaction container having a stirrer, a thermometer, and a nitrogen introducing pipe attached thereto, and a mixed solution of 745 g of 28% sodium methylate and 600 mL of methanol is dropped at a temperature of not more than 10° C. over 45 minutes. Subsequently, the solution is stirred for 50 minutes while the temperature is kept at 10° C. 1.6 kg of 0.1 mol/L hydrochloric acid is added to the reaction mixture to make the reaction solution acidic, and 3 L of water is further added to precipitate crystals. The crystals are filtered out, and washed with 2 L of water. Then, the crystals are dried under reduced pressure at 30° C. for 10 hours to obtain 702 g of 2-nitrobenzenesulfonic acid methyl ester.

WORKUP

后处理

  1. customis kept at 10° C
  2. customto precipitate crystals
  3. filtrationThe crystals are filtered out
  4. washwashed with 2 L of water
  5. customThen, the crystals are dried under reduced pressure at 30° C. for 10 hours