Glycerol → 3-Trityloxypropane-1,2-diol

HRID 724754

反応式

HRID 724754 の反応式
[OH:1][CH2:2][CH:3]([CH2:5][OH:6])[OH:4].[C:7](Cl)([C:20]1[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=1)([C:14]1[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=1)[C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=1>N1C=CC=CC=1>[C:7]([O:1][CH2:2][CH:3]([CH2:5][OH:6])[OH:4])([C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=1)([C:20]1[CH:21]=[CH:22][CH:23]=[CH:24][CH:25]=1)[C:14]1[CH:15]=[CH:16][CH:17]=[CH:18][CH:19]=1

参加物

4

反応物 2

HCID 753GlycerolHCID 6456Trityl chloride

生成物 1

HCID 28828273-Trityloxypropane-1,2-diol収率 59%

試薬・触媒・溶媒 1

HCID 1049Pyridine溶媒

実験手順

In 50 ml of pyridine was dissolved 4.6 g (50 mmol) of glycerol followed by addition of 13.9 g (50 mmol) of trityl chloride and the mixture was stirred at ambient temperature overnight. The reaction mixture was then concentrated under reduced pressure and the residue was diluted with water and extracted with ether. The organic layer was washed with water, dried over magnesium sulfate, and concentrated. The residue was purified by column chromatography (silica gel/chloroform-methanol) to provide 9.5 g (59%) of 1-O-tritylglycerol.

後処理

  1. concentrationThe reaction mixture was then concentrated under reduced pressure
  2. additionthe residue was diluted with water
  3. extractionextracted with ether
  4. washThe organic layer was washed with water
  5. dry with materialdried over magnesium sulfate
  6. concentrationconcentrated
  7. customThe residue was purified by column chromatography (silica gel/chloroform-methanol)

出典と根拠

ORDレコード
ord-33db2a77cdf744d0b4ea3f6b3d48e678
出典データセット
uspto-grants-1998_01
特許番号
US05705188

関連ノート

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