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Ammonium Chloride → 19-Tetrahydropyranyloxy-1,5-androstadiene-3,17-dione

HRID 1390736
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HRID 1390736 반응식
CC(C)([O-])C.[K+].[O:7]1[CH2:12][CH2:11][CH2:10][CH2:9][CH:8]1[O:13][CH2:14][C@@:15]12[C@@H:32]3[C@H:23]([C@H:24]4[C@@:28]([CH2:30][CH2:31]3)([CH3:29])[C:27](=[O:33])[CH2:26][CH2:25]4)[CH2:22][CH2:21][C:20]1=[CH:19][C:18](=[O:34])[CH:17]=[CH:16]2.[Cl-].[NH4+]>CS(C)=O>[O:7]1[CH2:12][CH2:11][CH2:10][CH2:9][CH:8]1[O:13][CH2:14][C@@:15]12[C@@H:32]3[C@H:23]([C@H:24]4[C@@:28]([CH2:30][CH2:31]3)([CH3:29])[C:27](=[O:33])[CH2:26][CH2:25]4)[CH2:22][CH:21]=[C:20]1[CH2:19][C:18](=[O:34])[CH:17]=[CH:16]2
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 25517Ammonium ChlorideHCID 2280690119-Tetrahydropyranyloxy-1,4-androstadiene-3,17-dioneHCID 23665647Potassium tert-butoxide

생성물 1

HCID 2280690219-Tetrahydropyranyloxy-1,5-androstadiene-3,17-dione

시약·촉매·용매 1

HCID 679Dimethyl Sulfoxide용매2회

실험 절차

To a solution of potassium t-butoxide in dimethylsulfoxide at 25° C. under nitrogen is added 19-tetrahydropyranyloxy-1,4-androstadiene-3,17-dione in dimethylsulfoxide with stirring. After 15 minutes the mixture is poured onto cold aqueous solution of ammonium chloride. The solid which forms is rapidly filtered, washed well with water and dissolved in ether. The ether solution is washed with water, dried over sodium sulfate and evaporated at room temperature to yield 19-tetrahydropyranyloxy-1,5-androstadiene-3,17-dione.

후처리

  1. filtrationThe solid which forms is rapidly filtered
  2. washwashed well with water
  3. dissolutiondissolved in ether
  4. washThe ether solution is washed with water
  5. dry with materialdried over sodium sulfate
  6. customevaporated at room temperature

출처 및 근거

ORD 기록
ord-0e0e7384f68941c4b02dda1f7564c6c4
출처 데이터셋
uspto-grants-1979_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04139617

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