Methyl Acrylate → Propanoic acid, 3-((2-methoxy-2-oxoethyl)thio)-, methyl ester
反応式
[C:1]([O:5][CH3:6])(=[O:4])[CH:2]=[CH2:3].[C:7]([O:11][CH3:12])(=[O:10])[CH2:8][SH:9].N1CCCCC1>>[CH3:6][O:5][C:1](=[O:4])[CH2:2][CH2:3][S:9][CH2:8][C:7]([O:11][CH3:12])=[O:10]参加物
4
反応条件
- 温度
- 50 °C
実験手順
Methyl acrylate (99.16 mL, 1.1 mol) was added slowly to a solution of methyl thioglycolate (91 mL, 1 mol) and piperidine (2 mL) while maintaining the temperature of reaction mixture at 50° C. The reaction mixture was stirred at 50° C. for 2 h. Excess methyl acrylate and piperidine were distilled off under high vacuum to yield 192 g (99%) of 3-methoxycarbonylmethylsulfanyl-propionic acid methyl ester as a colorless viscous oil. 1H NMR (400 MHz, CDCl3) δ 2.63 (d, J=7.2 Hz, 2H), 2.89 (d, J=7.2 Hz, 2H), 3.24 (s, 2H), 3.68 (s, 3H), 3.72 (s, 3H) ppm.
後処理
- temperaturewhile maintaining
- customthe temperature of reaction mixture at 50° C
- distillationExcess methyl acrylate and piperidine were distilled off under high vacuum
出典と根拠
- ORDレコード
- ord-66fa8b2735a34493a54cfd448e423691
- 出典データセット
- uspto-grants-2008_04
- 特許番号
- US07365200B2
反応ノート
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