반응 #50023

반응 방정식

trimethyl orthoformate

L-Proline

sulfuryl chloride

→

product

L-Proline Methyl Ester Hydrochloride

용매

methanol

반응 조건

후처리

1. 1
   workup.WAITAfter 16 hours at room temperature
2. 2
   온도another 4 hours at reflux
3. 3
   온도heating
4. 4
   온도at reflux
5. 5
   workup.WAITcontinued for another 24 hr
6. 6
   농축The reaction mixture was then concentrated
7. 7
   workup.WAITthe resultant oil was placed under high vacuum for several days

실험 절차

To a solution of L-Proline (115 g,1 mol) in methanol (1.2 L) at 0° C. was added sulfuryl chloride (45 mL, 0.55 mol) slowly during ~15-20 min, then the reaction mixture stirred overnight at room temperature. After 16 hours at room temperature and another 4 hours at reflux, trimethyl orthoformate (120 mL, 1.1 mol) was added and heating at reflux continued for another 24 hr. The reaction mixture was then concentrated and the resultant oil was placed under high vacuum for several days to afford the product as a clear oil (205 g).

출처