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Sodium Bicarbonate → HCID 11772697, 화합물

HRID 895840
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HRID 895840 반응식
[CH3:1][C:2]1([CH3:26])[C@@H:22]([OH:23])[CH2:21][CH2:20][C@@:19]2([CH3:24])[CH:3]1[CH2:4][CH2:5][C:6]1[C:7]3[C@:15]([CH3:25])([CH2:16][CH2:17][C:18]=12)[C@@H:10]([C@H:11]([CH3:14])[CH2:12][OH:13])[CH2:9][CH:8]=3.C(=O)(O)[O-].[Na+]>ClCCl>[OH:23][C@H:22]1[CH2:21][CH2:20][C@@:19]2([CH3:24])[CH:3]([CH2:4][CH2:5][C:6]3[C:7]4[C@:15]([CH3:25])([CH2:16][CH2:17][C:18]=32)[C@@H:10]([C@H:11]([CH3:14])[CH:12]=[O:13])[CH2:9][CH:8]=4)[C:2]1([CH3:1])[CH3:26]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 516892Sodium BicarbonateHCID 69283450HCID 69283450, 화합물

생성물 1

HCID 11772697HCID 11772697, 화합물수율 23.1%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

To a solution of 1 g (20S)-4,4,20-trimethyl-pregna-8,14-dien-3β,21-diol in 10 ml dichloromethane 5.4 ml of a 0.5 M Dess-Martin-Periodinane solution were added at room temperature. The mixture was stirred for one hour, poured into saturated sodium bicarbonate solution, extracted with ethyl acetate and washed with brine. The organic layer was dried over sodium sulfate, filtered and concentrated under reduced pressure. The residue was purified by column chromatography to give 230 mg (20S)-3β-hydroxy-4,4,20-trimethyl-pregna-8,14-dien-21-al as a white solid.

후처리

  1. extractionextracted with ethyl acetate
  2. washwashed with brine
  3. dry with materialThe organic layer was dried over sodium sulfate
  4. filtrationfiltered
  5. concentrationconcentrated under reduced pressure
  6. customThe residue was purified by column chromatography

출처 및 근거

ORD 기록
ord-d98242312ce7404ca37d2e755f2d56fe
출처 데이터셋
uspto-grants-2005_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06916921B2

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