HRID1388313

反应详情

EQUATION

反应方程式

HRID 1388313 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
110 °C

PROCEDURE

实验过程

A suspension of 800 mg of N,N',N"-tris[4-[[2,3,6-tri-O-acetyl-4-O-(2,3,4,6-tetra-O-acetyl-α-D-glucopyranosyl)-β-D-glucopyranosyl]oxy]phenyl]-1,3,5-benzenetrisulfonamide in 15 ml of methanol was cooled in an ice-water bath, then ammonia was bubbled in, with stirring for one hour. The cooling bath was removed and stirring was continued for 4 days. The solvents were evaporated and the residue was heated in vacuo at 110° C. for 2 hours. This residue was crystallized from a mixture of methanol and ethanol, giving 280 mg of the desired intermediate as a white powder, mp 206°-210° C.

WORKUP

后处理

  1. temperaturewas cooled in an ice-water bath
  2. customammonia was bubbled in,
  3. customThe cooling bath was removed
  4. stirringstirring
  5. waitwas continued for 4 days
  6. customThe solvents were evaporated
  7. customThis residue was crystallized from a mixture of methanol and ethanol