Methyl chloroformate → 3-Hydroxy-2-(hydroxymethyl)propyl methyl carbonate

HRID 1594623ノート

反応式

HRID 1594623 の反応式
[OH:1][CH2:2][CH:3]([CH2:6][OH:7])[CH2:4][OH:5].Cl[C:9]([O:11][CH3:12])=[O:10]>ClCCl.N1C=CC=CC=1>[CH3:12][O:11][C:9]([O:1][CH2:2][CH:3]([CH2:6][OH:7])[CH2:4][OH:5])=[O:10]

参加物

5

反応物 2

HCID 6586Methyl chloroformateHCID 78432Trimethylolmethane

生成物 1

HCID 222749913-Hydroxy-2-(hydroxymethyl)propyl methyl carbonate収率 42.1%

試薬・触媒・溶媒 2

HCID 1049Pyridine溶媒HCID 6344Dichloromethane溶媒

実験手順

To a solution of 2-(hydroxymethyl)-1,3-propanediol (9.4 mmol) in dichloromethane (20 mL) and pyridine (7.5 mL) at 0° C. was added methyl chloroformate (9.4 mmol) slowly. The resulting solution was warmed to room temperature and stirred for 16 h. The reaction was concentrated under reduced pressure and chromatographed by eluting with methanol-dichloromethane (1:4) to give 650 mg of 2-(methoxycarbonyloxymethyl)-1,3-propanediol.

後処理

  1. concentrationThe reaction was concentrated under reduced pressure
  2. customchromatographed
  3. washby eluting with methanol-dichloromethane (1:4)

出典と根拠

ORDレコード
ord-229c0332f800471186e76169b9bd5975
出典データセット
uspto-grants-2001_09
特許番号
US06284748B1

反応ノート

読み込み中…