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HRID1280862

反应详情

EQUATION

反应方程式

HRID 1280862 的结构方程式

REACTANTS

反应物

3
结构：O=S(=O)(O)O
HCID1118

Sulfuric acid

H2O4S

结构：CS(=O)(=O)Cl
HCID31297

Methanesulfonyl chloride

CH3ClO2S

结构：C[C@H](CCC(=O)O)[C@H]1CC[C@H]2[C@@H]3[C@H](O)C[C@@H]4C[C@H](O)CC[C@]4(C)[C@H]3C[C@H](O)[C@]12C
HCID221493

Cholic acid

C24H40O5

PRODUCTS

生成物

1
结构：CC(CCC(=O)O)C1CCC2C3C(O)CC4CC(OS(C)(=O)=O)CCC4(C)C3CC(O)C12C
HCID18425131

未命名化合物

AUXILIARIES

试剂、催化剂与溶剂

2
结构：O
溶剂HCID962

Water

H2O

结构：c1ccncc1
溶剂HCID1049

Pyridine

C5H5N

PROCEDURE

实验过程

100 g of cholic acid are dissolved in 500 ml of pyridine and 23.1 ml of mesyl chloride are added dropwise over a period of 30 minutes at 0° C. The mixture is stirred at RT for 3 hours, then poured into a solution of 400 ml of H2SO4 in 3 l of water at 0° C. and extracted 4 times using 750 ml of EA each time. The extract is dried over Na2SO4 and the solvent is removed in vacuo. The residue is crystallized using diisopropyl ether and 117.1 g are obtained; m.p. 121° C. (with decomposition).

WORKUP

后处理

  1. extractionextracted 4 times
  2. dry with materialThe extract is dried over Na2SO4
  3. customthe solvent is removed in vacuo
  4. customThe residue is crystallized
  5. customare obtained