Hydrochloric Acid → Ethyl 3-oxothiomorpholine-2-carboxylate
反応式
[NH:1]1[CH2:6][CH2:5][S:4][CH2:3][C:2]1=[O:7].C([N-]C(C)C)(C)C.[Li+].Cl[C:17]([O:19][CH2:20][CH3:21])=[O:18].Cl>O1CCCC1>[CH2:20]([O:19][C:17]([CH:3]1[S:4][CH2:5][CH2:6][NH:1][C:2]1=[O:7])=[O:18])[CH3:21]参加物
6
実験手順
A mixture of thiomorpholin-3-one (1 equivalent), tetrahydrofuran (5-40 parts), and lithium diisopropylamide (1-2 equivalents) is stirred at -10° to 50° C. for 1 to 3 hours. To this mixture is added ethyl chloroformate (1 to 2 equivalents). After 1 to 3 hours' stirring, the mixture is acidified with hydrochloric acid, concentrated, diluted with ethyl acetate, washed with water, dried, and concentrated to give 3-oxothiomorpholine-2-carboxylic acid ethyl ester in 80 to 90% yield.
後処理
- stirringAfter 1 to 3 hours' stirring
- concentrationconcentrated
- additiondiluted with ethyl acetate
- washwashed with water
- customdried
- concentrationconcentrated
出典と根拠
- ORDレコード
- ord-889881e554b3495c8d655e1a7038ac9b
- 出典データセット
- uspto-grants-1986_03
- 特許番号
- US04578378
反応ノート
読み込み中…