Trimethyl orthoformate → methyl L-prolinate hydrochloride
反応式
[NH:1]1[CH2:8][CH2:7][CH2:6][C@H:2]1[C:3]([OH:5])=[O:4].S(Cl)([Cl:12])(=O)=O.[CH:14](OC)(OC)OC>CO>[ClH:12].[CH3:14][O:4][C:3](=[O:5])[C@@H:2]1[CH2:6][CH2:7][CH2:8][NH:1]1参加物
5
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).
後処理
- waitAfter 16 hours at room temperature
- temperatureanother 4 hours at reflux
- temperatureheating
- temperatureat reflux
- waitcontinued for another 24 hr
- concentrationThe reaction mixture was then concentrated
- waitthe resultant oil was placed under high vacuum for several days
出典と根拠
- ORDレコード
- ord-597dbf67453e44ccb9afcd1128c217bb
- 出典データセット
- uspto-grants-1995_06
- 特許番号
- US05424444
反応ノート
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