Lithium Bromide → 21-Bromo-20-methyl-1alpha,3beta-diacetoxypregna-5,7-diene

HRID 1587635ノート

反応式

HRID 1587635 の反応式
[CH3:1][CH:2]([C@@H:15]1[C@:32]2([CH3:33])[C@H:18]([C:19]3[C@H:29]([CH2:30][CH2:31]2)[C@:27]2([CH3:28])[C:22]([CH2:23][C@@H:24]([O:38][C:39](=[O:41])[CH3:40])[CH2:25][C@@H:26]2[O:34][C:35](=[O:37])[CH3:36])=[CH:21][CH:20]=3)[CH2:17][CH2:16]1)[CH2:3]OS(C1C=CC(C)=CC=1)(=O)=O.[Br-:42].[Li+]>CC(C)=O>[Br:42][CH2:3][CH:2]([CH3:1])[C@@H:15]1[C@:32]2([CH3:33])[C@H:18]([C:19]3[C@H:29]([CH2:30][CH2:31]2)[C@:27]2([CH3:28])[C:22]([CH2:23][C@@H:24]([O:38][C:39](=[O:41])[CH3:40])[CH2:25][C@@H:26]2[O:34][C:35](=[O:37])[CH3:36])=[CH:21][CH:20]=3)[CH2:17][CH2:16]1

参加物

4

反応物 2

HCID 82050Lithium BromideHCID 8674694520-Methyl-1alpha,3beta-diacetoxy-21-p-toluenesulfonyloxypregna-5,7-diene

生成物 1

HCID 6778834921-Bromo-20-methyl-1alpha,3beta-diacetoxypregna-5,7-diene

試薬・触媒・溶媒 1

HCID 180Acetone溶媒

実験手順

To a solution of 51 mg of 20-methyl-1α,3β-diacetoxy-21-p-toluenesulfonyloxypregna-5,7-diene in 5 ml of acetone was added 100 mg of lithium bromide and the mixture was heated under reflux for 10 hours. The same isolation and purification procedure in Example 47 gave mg of 21-bromo-20-methyl-1α,3β-diacetoxypregna-5,7-diene, whose 1H NMR spectrum was identical with that obtained in Example 12.

後処理

  1. temperaturethe mixture was heated
  2. temperatureunder reflux for 10 hours
  3. customThe same isolation and purification procedure in Example 47

出典と根拠

ORDレコード
ord-60e7270ee4c24ea4a9764571a02f72fa
出典データセット
uspto-grants-1993_06
特許番号
US05218109

反応ノート

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