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

HRID 1063779ノート

反応式

HRID 1063779 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-0cb922e91b3c4a93b04716b1e583a6e2
出典データセット
uspto-grants-2005_11
特許番号
US06967193B1

反応ノート

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