Phosphate → 2-(2,4-Difluorophenyl)-1,2,3-propanetriol

HRID 1003774

반응식

HRID 1003774 반응식
[F:1][C:2]1[CH:7]=[C:6]([F:8])[CH:5]=[CH:4][C:3]=1[C:9]([OH:20])([CH2:15][O:16]C(=O)C)[CH2:10][O:11]C(=O)C.P([O-])([O-])([O-])=O>C1CCCCC1>[F:1][C:2]1[CH:7]=[C:6]([F:8])[CH:5]=[CH:4][C:3]=1[C:9]([OH:20])([CH2:15][OH:16])[CH2:10][OH:11]

참가 물질

4

반응물 2

HCID 1061PhosphateHCID 154634621,3-Diacetoxy-2-(2,4-difluorophenyl)-2-propanol

생성물 1

HCID 112179522-(2,4-Difluorophenyl)-1,2,3-propanetriol수율 93.2%

시약·촉매·용매 1

HCID 8078Cyclohexane용매

반응 조건

온도
30 °C

실험 절차

A 2 l reaction vessel was charged with 10 g of 2-(2,4-difluorophenyl)-1,3-diacetoxy-2-propanol, 2 g of Lipase AP-6 (made by Amano Pharmaceutical Co., Ltd., derived from Aspergillus niger, Enzyme No. 12), 500 ml of 50 mM phosphate buffer (pH 7.0) and 500 ml of cyclohexane. The resulting mixture was stirred at 30° C. for 24 hours. The reaction liquid was extracted three times with 1000 ml of ethyl acetate and dried over anhydrous sodium sulfate. The solvent was removed under reduced pressure and the residue was purified by column chromatography on silica gel (n-hexane/ethyl acetate=1/10) to give 6.6 g of 2-(2,4-difluorophenyl)-1,2,3-propanetriol.

후처리

  1. customA 2 l reaction vessel
  2. customThe reaction liquid
  3. extractionwas extracted three times with 1000 ml of ethyl acetate
  4. dry with materialdried over anhydrous sodium sulfate
  5. customThe solvent was removed under reduced pressure
  6. customthe residue was purified by column chromatography on silica gel (n-hexane/ethyl acetate=1/10)

출처 및 근거

ORD 기록
ord-80006c0af76c49e9b8b39335b0c8a6a0
출처 데이터셋
uspto-grants-2000_04
특허 번호
US06046354

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