Glycerol → 3-Trityloxypropane-1,2-diol

HRID 724754

반응식

HRID 724754 반응식
[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

참가 물질

4

반응물 2

HCID 753GlycerolHCID 6456Trityl chloride

생성물 1

HCID 28828273-Trityloxypropane-1,2-diol수율 59%

시약·촉매·용매 1

HCID 1049Pyridine용매

실험 절차

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.

후처리

  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)

출처 및 근거

ORD 기록
ord-33db2a77cdf744d0b4ea3f6b3d48e678
출처 데이터셋
uspto-grants-1998_01
특허 번호
US05705188

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