Pyridinium → HCID 86748908, 화합물

HRID 1735742노트

반응식

HRID 1735742 반응식
[NH+]1C=CC=CC=1.[OH:7][C@H:8]1[CH2:25][CH2:24][C@@:23]2([CH3:26])[C@H:10]([CH2:11][CH2:12][C@@H:13]3[C@@H:22]2[CH2:21][CH2:20][C@@:18]2([CH3:19])[C@:14]3([OH:29])[CH2:15][CH2:16][C@@H:17]2[CH:27]=[O:28])[CH2:9]1>ClCCl.C(OCC)C>[O:7]=[C:8]1[CH2:25][CH2:24][C@@:23]2([CH3:26])[C@H:10]([CH2:11][CH2:12][C@@H:13]3[C@@H:22]2[CH2:21][CH2:20][C@@:18]2([CH3:19])[C@:14]3([OH:29])[CH2:15][CH2:16][C@@H:17]2[CH:27]=[O:28])[CH2:9]1

참가 물질

5

반응물 2

HCID 4989215PyridiniumHCID 109033043beta,14beta-Dihydroxy-5beta-androstane-17beta-carboxaldehyde

생성물 1

HCID 86748908HCID 86748908, 화합물수율 60.4%

시약·촉매·용매 2

HCID 3283Diethyl Ether용매HCID 6344Dichloromethane용매2회

실험 절차

To a suspension of 0.88 g of pyridinium dicromate in 2.2 ml of dichloromethane a solution of 0.50 g of 3β,14β-dihydroxy-5β-androstane-17β-carboxaldehyde (Boutagy J. and Thomas R., Aust. J. Chem., 1971, 24, 2723) in 2.5 ml of dichloromethane was added at room temperature. After 20 hrs the mixture was diluted with diethyl ether and filtered through celite; the filtrate was evaporated to dryness under reduced pressure. The crude product was purified by flash-chromatography (SiO2) using n-hexane/ethyl acetate 6/4 as eluant; the fractions containing the title compound were collected and evaporated to give 0.30 g of the title compound (II-e) as a white foam.

후처리

  1. additionwas added at room temperature
  2. filtrationfiltered through celite
  3. customthe filtrate was evaporated to dryness under reduced pressure
  4. customThe crude product was purified by flash-chromatography (SiO2)
  5. additionthe fractions containing the title compound
  6. customwere collected
  7. customevaporated

출처 및 근거

ORD 기록
ord-480f0e896c874bd8aec6782c4f7528c3
출처 데이터셋
uspto-grants-1996_07
특허 번호
US05538960

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