تفاعل #481599
ord-3eb8d0f494364333b92057c4088f6fd1
معادلة التفاعل
thionyl chloride
4-hydroxyproline
ethanol
→
4hydroxy-L-proline ethyl ester hydrochloride
المتفاعلات
الكواشف
لا شيء
ظروف التفاعل
الظروف التفصيلية
See reaction.notes.procedure_details.
المعالجة
- 1أخرىequipped with an addition funnel
- 2درجة الحرارةThe flask was then cooled in a dry ice/acetone bath
- 3أخرىThe funnel was removed
- 4أخرىThe flask was equipped with a reflux condenser and a sodium hydroxide trap
- 5درجة الحرارةthe mixture was refluxed for two hours
- 6أخرىThe product was precipitated in ether
- 7أخرىisolated by filtration
- 8غسيلwashed three times with ether
- 9أخرىit was dried under a stream of nitrogen
الإجراء التجريبي
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.