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

HRID 1587635노트

반응식

HRID 1587635 반응식
[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

참가 물질

4

반응물 2

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

생성물 1

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

시약·촉매·용매 1

HCID 180Acetone용매

실험 절차

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.

후처리

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

출처 및 근거

ORD 기록
ord-60e7270ee4c24ea4a9764571a02f72fa
출처 데이터셋
uspto-grants-1993_06
특허 번호
US05218109

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