Lithium Chloride → 16alpha-Allyloxy-21-chloro-11beta,17-dihydroxypregn-4-ene-3,20-dione

HRID 918413노트

반응식

HRID 918413 반응식
[CH2:1]([O:4][C@@H:5]1[CH2:25][C@@H:24]2[C@:11]([CH3:29])([CH2:12][C@H:13]([OH:28])[C@H:14]3[C@H:23]2[CH2:22][CH2:21][C:20]2[C@:15]3([CH3:27])[CH2:16][CH2:17][C:18](=[O:26])[CH:19]=2)[C@@:6]1([OH:30])[C:7](=[O:10])[CH2:8]O)[CH:2]=[CH2:3].[Cl-:31].[Li+]>CN(C)C=O.O>[CH2:1]([O:4][C@@H:5]1[CH2:25][C@@H:24]2[C@:11]([CH3:29])([CH2:12][C@H:13]([OH:28])[C@H:14]3[C@H:23]2[CH2:22][CH2:21][C:20]2[C@:15]3([CH3:27])[CH2:16][CH2:17][C:18](=[O:26])[CH:19]=2)[C@@:6]1([OH:30])[C:7](=[O:10])[CH2:8][Cl:31])[CH:2]=[CH2:3]

참가 물질

5

반응물 2

HCID 433294Lithium ChlorideHCID 6814270016alpha-Allyloxy-11beta,17,21-trihydroxypregn-4-ene-3,20-dione

생성물 1

HCID 8673375816alpha-Allyloxy-21-chloro-11beta,17-dihydroxypregn-4-ene-3,20-dione

시약·촉매·용매 2

HCID 962Water용매HCID 6228Dimethylformamide용매

실험 절차

A solution of 16α-allyloxy-11β,17,21-trihydroxypregn-4-ene-3,20-dione, 21-methanesulfonate (4.6 mmoles) in 60 ml of dimethylformamide is refluxed for 1 hour under nitrogen with 5 g of lithium chloride. The solution is cooled, diluted with water and filtered. The solid is dissolved in chloroform, washed with 5% hydrochloric acid, water, dried, and evaporated in vacuo to yield the title compound.

후처리

  1. temperatureThe solution is cooled
  2. filtrationfiltered
  3. dissolutionThe solid is dissolved in chloroform
  4. washwashed with 5% hydrochloric acid, water
  5. customdried
  6. customevaporated in vacuo

출처 및 근거

ORD 기록
ord-79021aae87324b95954e1d69ef5b21f0
출처 데이터셋
uspto-grants-1976_07
특허 번호
US03971773

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