huagongshe.com
HRID1439627

反应详情

EQUATION

反应方程式

HRID 1439627 的结构方程式

REACTANTS

反应物

3
结构：Cl.Cl.NCCSSCCN
HCID5941

2,2'-Dithiodi(ethylammonium) dichloride

C4H14Cl2N2S2

结构：C(=NC1CCCCC1)=NC1CCCCC1
HCID10868

Dicyclohexylcarbodiimide

C13H22N2

结构：CC(C)(CO)[C@@H](O)C(=O)NCCC(=O)[O-].CC(C)(CO)[C@@H](O)C(=O)NCCC(=O)[O-].[Ca+2]
HCID443753

Calcium pantothenate

C18H32CaN2O10

PRODUCTS

生成物

1
结构：CC(C)(CO)[C@@H](O)C(=O)NCCC(=O)NCCSSCCNC(=O)CCNC(=O)[C@H](O)C(C)(C)CO
HCID452306

Pantethine

C22H42N4O8S2

收率 69.2%

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

2 次

PROCEDURE

实验过程

11.9g. of calcium pantothenate, 6.8g. of cystamine dihydrochloride and 7.7g. of 1-hydroxylbenzotrizole were dissolved in 50ml. of pyridine and 10ml. of water, and thereafter pyridine (25ml.) solution of 10.5g. of dicyclohexylcarbodiimide was added thereto at a time, and the reaction was effected at a temperature below 10° C for 1 hour and then for 5 hours at a room temperature. Next the solvent was removed under a reduced pressure, the residue thereof was added with 50ml. of water, and the deposited crystals were removed by filtration. Pyridine left in the filtered mother liquor was completely removed azetropically with water. The residue thereof was added with 50ml. of water and after cooling, the deposited crystals were filtration removed and extracted with 20ml. of chloroform two times. The water layer was treated under a reduced pressure to remove the remaining chloroform, and thereafter like Example 1, passed through the ion exchange resin, and the flowed out liquid was concentrated under a reduced pressure and thereby colorless transparent viscous liquid of pantethine which was the objective compound was obtained. Drying was carried out by means of a vacuum dryer for one night and as a result 9.6g. of pantethine (yield rate 69.2%) was obtained.

WORKUP

后处理

  1. dissolutionof 1-hydroxylbenzotrizole were dissolved in 50ml
  2. waitfor 5 hours at a room temperature
  3. customNext the solvent was removed under a reduced pressure
  4. additionthe residue thereof was added with 50ml
  5. customof water, and the deposited crystals were removed by filtration
  6. waitPyridine left in the filtered mother liquor
  7. customwas completely removed azetropically with water
  8. additionThe residue thereof was added with 50ml
  9. temperatureof water and after cooling
  10. filtrationfiltration
  11. customremoved
  12. extractionextracted with 20ml
  13. additionThe water layer was treated under a reduced pressure
  14. customto remove the remaining chloroform
  15. concentrationwas concentrated under a reduced pressure
  16. customwas obtained
  17. customDrying
  18. waitwas carried out by means of a vacuum dryer for one night and as a result 9.6g