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1,3-Dibromo-5,5-dimethylhydantoin → 3beta,24-Bis(tert-butyldimethylsilyloxy)-4,4-dimethylchola-5,7-diene

HRID 1764956
ノート
印刷プレビュー

反応式

HRID 1764956 の反応式
[Si:1]([O:8][C@H:9]1[CH2:38][CH2:37][C@@:36]2([CH3:39])[C:11](=[CH:12][CH2:13][C@@H:14]3[C@@H:35]2[CH2:34][CH2:33][C@@:32]2([CH3:40])[C@H:15]3[CH2:16][CH2:17][C@@H:18]2[C@H:19]([CH3:31])[CH2:20][CH2:21][CH2:22][O:23][Si:24]([C:27]([CH3:30])([CH3:29])[CH3:28])([CH3:26])[CH3:25])[C:10]1([CH3:42])[CH3:41])([C:4]([CH3:7])([CH3:6])[CH3:5])([CH3:3])[CH3:2].BrN1C(C)(C)C(=O)N(Br)C1=O>CCCCCC.C1C=CC=CC=1>[Si:1]([O:8][C@H:9]1[CH2:38][CH2:37][C@@:36]2([CH3:39])[C:11](=[CH:12][CH:13]=[C:14]3[C@@H:35]2[CH2:34][CH2:33][C@@:32]2([CH3:40])[C@H:15]3[CH2:16][CH2:17][C@@H:18]2[C@H:19]([CH3:31])[CH2:20][CH2:21][CH2:22][O:23][Si:24]([C:27]([CH3:28])([CH3:29])[CH3:30])([CH3:26])[CH3:25])[C:10]1([CH3:41])[CH3:42])([C:4]([CH3:5])([CH3:6])[CH3:7])([CH3:3])[CH3:2]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 2

HCID 64791,3-Dibromo-5,5-dimethylhydantoinHCID 155430903beta,24-Bis(tert-butyldimethylsilyloxy)4,4-dimethylchol-5-ene

生成物 1

HCID 694129983beta,24-Bis(tert-butyldimethylsilyloxy)-4,4-dimethylchola-5,7-diene収率 88.9%

試薬・触媒・溶媒 2

HCID 241Benzene溶媒HCID 8058Hexane
溶媒

実験手順

3β,24-Bis(tert-butyldimethylsilyloxy)-4,4-dimethylchol-5-ene (44 g) is dissolved in a warm mixture of hexane (2 l) and benzene (540 ml). 1,3-Dibromo-5,5-dimethylhydantoin (15.32 g) is added and the mixture is refluxed for 20 min and then cooled rapidly to room temperature, and the insoluble material is removed by filtration. The filtrate is concentrated under reduced pressure and o-xylene (2 l) and quinaldine (84 ml) is added. The mixture is refluxed for 1 hour. After aqueous work-up and trituration with methanol, 3β,24-bis (tert-butyldimethylsilyloxy)-4,4-dimethylchola-5,7-diene (39 g) is isolated. Melting point: 98-106° C. 1H-NMR (CDCl3, 400 MHz): δ=5.9 (1H, m); 5.54 (1H, m); 3.58 (2H, m); 3.35 (1H, m); 0.91 (18H, s); 0.05 (12H, m).

後処理

  1. temperaturethe mixture is refluxed for 20 min
  2. customthe insoluble material is removed by filtration
  3. concentrationThe filtrate is concentrated under reduced pressure and o-xylene (2 l) and quinaldine (84 ml)
  4. additionis added
  5. temperatureThe mixture is refluxed for 1 hour

出典と根拠

ORDレコード
ord-576a977ce06f4ae98d24808f644a1451
出典データセット
uspto-grants-2007_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
USRE039678E1

反応ノート

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