Реакция #1526809

Уравнение реакции

calcium pantothenate

cystamine dihydrochloride

dicyclohexylcarbodiimide

→

pantethine

Выход 69.2%

Растворители

pyridine

pyridine

water

Условия реакции

Обработка

1. 1
   workup.DISSOLUTIONof 1-hydroxylbenzotrizole were dissolved in 50ml
2. 2
   workup.WAITfor 5 hours at a room temperature
3. 3
   ДругоеNext the solvent was removed under a reduced pressure
4. 4
   workup.ADDITIONthe residue thereof was added with 50ml
5. 5
   Другоеof water, and the deposited crystals were removed by filtration
6. 6
   workup.WAITPyridine left in the filtered mother liquor
7. 7
   Другоеwas completely removed azetropically with water
8. 8
   workup.ADDITIONThe residue thereof was added with 50ml
9. 9
   Температураof water and after cooling
10. 10
    Фильтрацияfiltration
11. 11
    Другоеremoved
12. 12
    Экстракцияextracted with 20ml
13. 13
    workup.ADDITIONThe water layer was treated under a reduced pressure
14. 14
    Другоеto remove the remaining chloroform
15. 15
    Концентрированиеwas concentrated under a reduced pressure
16. 16
    Другоеwas obtained
17. 17
    ДругоеDrying
18. 18
    workup.WAITwas carried out by means of a vacuum dryer for one night and as a result 9.6g

Методика

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.

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