反応 #50023

反応方程式

trimethyl orthoformate

L-Proline

sulfuryl chloride

→

product

L-Proline Methyl Ester Hydrochloride

溶媒

methanol

反応条件

後処理

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

実験手順

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).

出典