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Tetrahydrofuran → 1alpha,3beta-Bis(tert-butyldimethylsilyloxy)-17-methyleneandrost-5-ene

HRID 1792221
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HRID 1792221 반응식
O1CCC[CH2:2]1.CC(C)([O-])C.[K+].[Si:12]([O:19][C@@H:20]1[C@@:37]2([CH3:38])[C:24](=[CH:25][CH2:26][C@@H:27]3[C@@H:36]2[CH2:35][CH2:34][C@@:32]2([CH3:33])[C@H:28]3[CH2:29][CH2:30][CH2:31]2)[CH2:23][C@@H:22]([O:39][Si:40]([C:43]([CH3:46])([CH3:45])[CH3:44])([CH3:42])[CH3:41])[CH2:21]1)([C:15]([CH3:18])([CH3:17])[CH3:16])([CH3:14])[CH3:13]>[Br-].C[P+](C1C=CC=CC=1)(C1C=CC=CC=1)C1C=CC=CC=1.CC(C)=O.CO.CCCCCC.O>[Si:12]([O:19][C@@H:20]1[C@@:37]2([CH3:38])[C:24](=[CH:25][CH2:26][C@@H:27]3[C@@H:36]2[CH2:35][CH2:34][C@@:32]2([CH3:33])[C@H:28]3[CH2:29][CH2:30][C:31]2=[CH2:2])[CH2:23][C@@H:22]([O:39][Si:40]([C:43]([CH3:46])([CH3:45])[CH3:44])([CH3:41])[CH3:42])[CH2:21]1)([C:15]([CH3:18])([CH3:17])[CH3:16])([CH3:14])[CH3:13]
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참가 물질

9

반응물 3

HCID 8028Tetrahydrofuran2회HCID 23665647Potassium tert-butoxideHCID 696305411alpha,3beta-Bis(tert-butyldimethylsilyloxy)androst-5-ene

생성물 1

HCID 696308851alpha,3beta-Bis(tert-butyldimethylsilyloxy)-17-methyleneandrost-5-ene

시약·촉매·용매 5

HCID 74505Methyltriphenyliphosphonium bromide
촉매
HCID 180Acetone용매
HCID 887Methanol용매
HCID 962Water용매
HCID 8058Hexane용매2회

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온도
60 °C

실험 절차

A mixture of tetrahydrofuran (70 ml), methyltriphenylphosphonium bromide (50 g) and potassium t-butoxide (13.9 g) were stirred at 60° C. for 2 hours, while under suspension. To this suspension, was added 1α,3β-bis(tert-butyldimethylsilyloxy)androst-5-ene (18.7 g) and tetrahydrofuran (60 ml), followed by reaction for 2 hours under reflux. Under cooling with ice, the reaction mixture was slowly added to a cooled mixture of hexane (200 ml) and water (100 ml) to stop the reaction. The organic layer was washed with saturated brine twice, dried over anhydrous magnesium sulfate and evaporated under reduced pressure to remove the solvent, giving crude crystals (27 g). The crude crystals were mixed with hexane (100 ml), stirred at room temperature while under suspension. After filtering off insoluble material from the suspension, the filtrate was evaporated under reduced pressure to remove the solvent, giving crude crystals, which were then dissolved in acetone (80 ml) by stirring at room temperature. The mixture was mixed with methanol (160 ml) and stirred at room temperature; the thus precipitated crystals were collected by filtration and dried to give the titled compound (13.2 g).

후처리

  1. customfollowed by reaction for 2 hours
  2. temperatureunder reflux
  3. temperatureUnder cooling with ice
  4. customthe reaction
  5. washThe organic layer was washed with saturated brine twice
  6. dry with materialdried over anhydrous magnesium sulfate
  7. customevaporated under reduced pressure
  8. customto remove the solvent
  9. customgiving crude crystals (27 g)
  10. stirringstirred at room temperature while under suspension
  11. filtrationAfter filtering off insoluble material from the suspension
  12. customthe filtrate was evaporated under reduced pressure
  13. customto remove the solvent
  14. customgiving crude crystals, which
  15. stirringby stirring at room temperature
  16. stirringstirred at room temperature
  17. filtrationthe thus precipitated crystals were collected by filtration
  18. customdried

출처 및 근거

ORD 기록
ord-cf7db74464e144219f9c73c4d6f70138
출처 데이터셋
uspto-grants-2006_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07074777B2

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