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HRID1112196

反应详情

EQUATION

反应方程式

HRID 1112196 的结构方程式

REACTANTS

反应物

2
结构：O=S(=O)(Cl)c1cc(S(=O)(=O)Cl)cc(S(=O)(=O)Cl)c1
HCID88940

1,3,5-Benzenetrisulfonyl trichloride

C6H3Cl3O6S3

结构：CC(=O)OC[C@H]1OC(OC(C)=O)[C@H](N)[C@@H](OC(C)=O)[C@@H]1OC(C)=O
HCID13059363

未命名化合物

PRODUCTS

生成物

1
结构：N[C@@H]1[C@@H](O)[C@H](O)[C@@H](CO)OC1(O)S(=O)(=O)c1cc(S(=O)(=O)C2(O)O[C@H](CO)[C@@H](O)[C@H](O)[C@H]2N)cc(S(=O)(=O)C2(O)O[C@H](CO)[C@@H](O)[C@H](O)[C@H]2N)c1
HCID131711300

未命名化合物

AUXILIARIES

试剂、催化剂与溶剂

1
结构：CC#N.c1ccncc1
溶剂HCID21959178

未命名化合物

PROCEDURE

实验过程

The novel intermediate benzene 1,3,5-trisulfonyl trisglucosamine compound is prepared by reacting tetra-O-acetyl glucosamine (II) with 1,3,5-benzenetrisulfonyl chloride in a weakly basic polar medium such as acetonitrile-pyridine for 24 hours. The solvent is concentrated and the tetraacetyl trisulfonyl derivative (III) is precipitated from ice water and extracted into methylene dichloride. The solvent is evaporated and the material is dissolved in cold methanol saturated with ammonia. Standing in the cold for 24 hours, followed by the addition of nitrogen gas to remove ammonia, produces a thick oil (IV) on evaporation. The oil is purified from water with activated charcoal, filtration and drying to give the intermediate glucopyranose.

WORKUP

后处理

  1. customfor 24 hours
  2. concentrationThe solvent is concentrated
  3. customthe tetraacetyl trisulfonyl derivative (III) is precipitated from ice water
  4. extractionextracted into methylene dichloride
  5. customThe solvent is evaporated
  6. dissolutionthe material is dissolved in cold methanol saturated with ammonia
  7. customcold for 24 hours
  8. additionfollowed by the addition of nitrogen gas
  9. customto remove ammonia