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17,21-Bis(acetyloxy)pregn-4-ene-3,20-dione → 17,21-Diacetoxy-6-methylene-4-pregnene-3,20-dione

HRID 2059159
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인쇄 미리보기

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HRID 2059159 반응식
[C:1]([O-])(=O)C.[Na+].[C:6]([O:9][C@:10]1([C@:34]2([CH3:35])[C@H:20]([C@H:21]3[C@H:31]([CH2:32][CH2:33]2)[C@:29]2([CH3:30])[C:24](=[CH:25][C:26](=[O:36])[CH2:27][CH2:28]2)[CH2:23][CH2:22]3)[CH2:19][CH2:18]1)[C:11](=[O:17])[CH2:12][O:13][C:14](=[O:16])[CH3:15])(=[O:8])[CH3:7]>C(Cl)Cl.COCOC.P(Cl)(Cl)(Cl)=O.O>[C:6]([O:9][C@:10]1([C@:34]2([CH3:35])[C@H:20]([C@H:21]3[C@H:31]([CH2:32][CH2:33]2)[C@:29]2([CH3:30])[C:24](=[CH:25][C:26](=[O:36])[CH2:27][CH2:28]2)[C:23](=[CH2:1])[CH2:22]3)[CH2:19][CH2:18]1)[C:11](=[O:17])[CH2:12][O:13][C:14](=[O:16])[CH3:15])(=[O:8])[CH3:7]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 2

HCID 10216517,21-Bis(acetyloxy)pregn-4-ene-3,20-dioneHCID 517045Sodium Acetate

생성물 1

HCID 1295177117,21-Diacetoxy-6-methylene-4-pregnene-3,20-dione수율 80.3%

시약·촉매·용매 4

HCID 962Water용매HCID 6344Dichloromethane용매2회
HCID 8020
Dimethoxymethane
용매
HCID 24813Phosphorus oxychloride용매

실험 절차

A suspension of 1.0 g of sodium acetate in 30 ml of methylene chloride, 30 ml of formaldehyde dimethylacetal and 3.8 ml of phosphorus oxychloride is combined with 1.0 g of 17,21-diacetoxy-4-pregnene-3,20-dione and refluxed for 35 hours under agitation. After cooling to room temperature, the mixture is diluted with methylene chloride and water. Under stirring, a saturated soda solution is added dropwise until an alkaline reaction of the aqueous phase has been obtained. The organic phase is separated, washed with water, dried over sodium sulfate, and evaporated under vacuum. Finally, the product is recrystallized from acetone/hexane, thus isolating 825 mg of 17,21-diacetoxy-6-methylene-4-pregnene-3,20-dione, mp 227°-228° C.

후처리

  1. temperaturerefluxed for 35 hours under agitation
  2. additiona saturated soda solution is added dropwise until an alkaline reaction of the aqueous phase
  3. customhas been obtained
  4. customThe organic phase is separated
  5. washwashed with water
  6. dry with materialdried over sodium sulfate
  7. customevaporated under vacuum
  8. customFinally, the product is recrystallized from acetone/hexane

출처 및 근거

ORD 기록
ord-094349ab36a643188f1add06d1972016
출처 데이터셋
uspto-grants-1982_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04322349

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