Water → MS-1254
反応式
C[O-].[Na+].[CH3:4][O:5][C:6](=[O:9])[CH2:7][SH:8].Cl[CH2:11][C:12](=[O:14])[CH3:13].O>CO>[CH3:4][O:5][C:6](=[O:9])[CH2:7][S:8][CH2:11][C:12](=[O:14])[CH3:13]参加物
6
実験手順
To a mixture of a 5.4 M methanolic solution of sodium methylate (185 mL, 1.00 mol) in 500 mL methanol is added mercapto-acetic acid methyl ester (97.0 g, 912 mmol) at RT. After stirring for 20 minutes at RT chloro acetone (80 mL, 1.0 mmol) is added carefully. After complete addition the reaction mixture is heated at reflux for 20 minutes. The reaction mixture is added to water and extracted with diethyl ether. The organic layer is washed with brine, dried over Na2SO4 and the solvent is evaporated under reduced pressure. The crude reaction product is distilled under reduced pressure (75° C.-90° C., 0.3 mbar) yielding the desired product as colorless liquid. Yield: 61.5 g. (M+H)+=163
後処理
- additionis added carefully
- additionAfter complete addition the reaction mixture
- temperatureis heated
- temperatureat reflux for 20 minutes
- extractionextracted with diethyl ether
- washThe organic layer is washed with brine
- dry with materialdried over Na2SO4
- customthe solvent is evaporated under reduced pressure
- customThe crude reaction product
- distillationis distilled under reduced pressure (75° C.-90° C., 0.3 mbar)
出典と根拠
- ORDレコード
- ord-476cc25d823746b4ae7c75845e272c55
- 出典データセット
- uspto-grants-2016_01
- 特許番号
- US09243000B2
反応ノート
読み込み中…