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

HRID 918413ノート

反応式

HRID 918413 の反応式
[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]

参加物

5

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 6228Dimethylformamide溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-79021aae87324b95954e1d69ef5b21f0
出典データセット
uspto-grants-1976_07
特許番号
US03971773

反応ノート

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