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Potassium Acetate → 3beta-Hydroxycholest-5-en-24-one acetate

HRID 1448022
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HRID 1448022 반응식
Cl[CH:2]1[CH2:27][CH2:26][C@@:25]2([CH3:28])[C:4](=[CH:5][CH2:6][C@@H:7]3[C@@H:24]2[CH2:23][CH2:22][C@@:21]2([CH3:29])[C@H:8]3[CH2:9][CH2:10][C@@H:11]2[C@H:12]([CH3:20])[CH2:13][CH2:14][C:15](=[O:19])[CH:16]([CH3:18])[CH3:17])[CH2:3]1.[C:30]([O-:33])(=[O:32])[CH3:31].[K+]>C(O)(=O)C>[C:30]([OH:33])(=[O:32])[CH3:31].[OH:32][C@H:2]1[CH2:27][CH2:26][C@@:25]2([CH3:28])[C:4](=[CH:5][CH2:6][C@@H:7]3[C@@H:24]2[CH2:23][CH2:22][C@@:21]2([CH3:29])[C@H:8]3[CH2:9][CH2:10][C@@H:11]2[C@H:12]([CH3:20])[CH2:13][CH2:14][C:15](=[O:19])[CH:16]([CH3:18])[CH3:17])[CH2:3]1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 517044Potassium AcetateHCID 542306963-Chlorocholest-5-en-24-one

생성물 1

HCID 867367383beta-Hydroxycholest-5-en-24-one acetate

시약·촉매·용매 1

HCID 176Acetic Acid용매

실험 절차

To the solution of 3-chlorocholest-5-en-24-one in glacial acetic acid (3 ml) was added anhydrous potassium acetate (0.2 g) and the solution was refluxed for 4 hours. The reaction mixture was concentrated and extracted with diethyl ether. The ether layer was washed with water, dried over magnesium sulfate and evaporated. The residue was chromatographed on silica gel to give 81.1 mg of 3β-hydroxycholest-5-en-24-one acetate having a melting point of 125°-127° C. after recrystallization from methanol.

후처리

  1. temperaturethe solution was refluxed for 4 hours
  2. concentrationThe reaction mixture was concentrated
  3. extractionextracted with diethyl ether
  4. washThe ether layer was washed with water
  5. dry with materialdried over magnesium sulfate
  6. customevaporated
  7. customThe residue was chromatographed on silica gel

출처 및 근거

ORD 기록
ord-730a62660bc549989b501917ac969219
출처 데이터셋
uspto-grants-1979_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04179452

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