반응 #481599

반응 방정식

thionyl chloride

4-hydroxyproline

ethanol

→

4hydroxy-L-proline ethyl ester hydrochloride

반응 조건

후처리

1. 1
   기타equipped with an addition funnel
2. 2
   온도The flask was then cooled in a dry ice/acetone bath
3. 3
   기타The funnel was removed
4. 4
   기타The flask was equipped with a reflux condenser and a sodium hydroxide trap
5. 5
   온도the mixture was refluxed for two hours
6. 6
   기타The product was precipitated in ether
7. 7
   기타isolated by filtration
8. 8
   세척washed three times with ether
9. 9
   기타it was dried under a stream of nitrogen

실험 절차

200 mL of absolute ethanol were placed in a 500-mL one-necked round-bottomed flask equipped with an addition funnel. The flask was then cooled in a dry ice/acetone bath, then 17 mL (0.23 mmoles) of thionyl chloride were added from the addition funnel over a 10 minute period. The funnel was removed, and 26.2 g (0.20 mmoles) of 4-hydroxyproline were added in one portion while stirring. The flask was equipped with a reflux condenser and a sodium hydroxide trap, and the mixture was refluxed for two hours. The product was precipitated in ether, isolated by filtration, and washed three times with ether, then it was dried under a stream of nitrogen followed by high vacuum.

출처