HRID903614

反应详情

EQUATION

反应方程式

HRID 903614 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To a mixture of about 3.0 grams of 2,3,4,6-tetra-O-acetyl-α-D-mannopyranosyl azide, 0.5 grams Raney nickel catalyst, and 40 ml. ethyl acetate, is vigorously agitated with hydrogen at atmospheric pressure, at a temperature of about 25° C. for a period of about 6.5 hours. The reaction mixture is filtered through diatomaceous silica, and the filtered solution is evaporated in vacuo to a syrup which crystallizes upon standing at a temperature of about 5° C. The crystalline product is recrystallized from 2-propanol to give about 1.7 grams of 2,3,4,6-tetra-O-acetyl-β-D-mannopyranosylamine; m.p. 145°-147° C.; [α]D25 -9.8° (c 1.02, methanol).

WORKUP

后处理

  1. filtrationThe reaction mixture is filtered through diatomaceous silica
  2. customthe filtered solution is evaporated in vacuo to a syrup which
  3. customcrystallizes
  4. customupon standing at a temperature of about 5° C
  5. customThe crystalline product is recrystallized from 2-propanol