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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
ノート
印刷プレビュー

反応式

HRID 2059159 の反応式
[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]
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 4

HCID 962Water溶媒HCID 6344Dichloromethane溶媒2 回
HCID 8020
Dimethoxymethane
溶媒
HCID 24813Phosphorus oxychloride溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-094349ab36a643188f1add06d1972016
出典データセット
uspto-grants-1982_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04322349

反応ノート

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