HRID580086

反应详情

EQUATION

反应方程式

HRID 580086 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

33.2 g (0.2 mol) of this m-nitrobenzaldoxime, 70 g (0.35 mol) of a 50% aqueous solution of phosphoric acid, 0.3 g of a 10% Pt-C catalyst and 300 ml of isobutanol were charged into a hermetically sealed glass container and vigorously stirred while charging hydrogen. Reaction was continued at temperatures of 25° to 30° C. for 18 hours and 23 l of hydrogen was absorbed. The reaction mixture from which crystals deposited was filtered and 54.8 g of crude m-aminobenzylamine phosphoric acid salt (yield 86.1%) was obtained. This crude m-aminobenzylamine phosphoric acid salt was recrystallized from a 50% methanol-water solution and pure m-aminobenzylamine phosphoric acid salt of white and flaky crystals was obtained. M.P. 210°-213° C.

WORKUP

后处理

  1. customReaction
  2. custom23 l of hydrogen was absorbed
  3. filtrationThe reaction mixture from which crystals deposited was filtered