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Sulfuric Acid → HCID 15871124, 화합물

HRID 2187287
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HRID 2187287 반응식
[CH3:1][CH:2]([CH2:4][CH2:5][CH2:6][C@H:7]([C@@H:9]1[C@:26]2([CH3:27])[C@H:12]([C:13]3[CH2:14][CH:15]=[C:16]4[C@:21]([C:23]=3[CH2:24][CH2:25]2)([CH3:22])[CH2:20][CH2:19][C@H:18]([OH:28])[CH2:17]4)[CH2:11][CH2:10]1)[CH3:8])[CH3:3].CC(C)[O-].[Al+3].CC(C)[O-].CC(C)[O-].S(=O)(=O)(O)O>C1(C)C=CC=CC=1.C1(=O)CCCCC1>[CH3:3][CH:2]([CH2:4][CH2:5][CH2:6][C@H:7]([C@@H:9]1[C@:26]2([CH3:27])[C@H:12]([C:13]3[CH2:14][CH2:15][C:16]4[C@:21]([C:23]=3[CH2:24][CH2:25]2)([CH3:22])[CH2:20][CH2:19][C:18](=[O:28])[CH:17]=4)[CH2:11][CH2:10]1)[CH3:8])[CH3:1]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 3

HCID 1118Sulfuric AcidHCID 11143Aluminum isopropoxideHCID 1298468-Dehydrocholesterol

생성물 1

HCID 15871124HCID 15871124, 화합물수율 69.9%

시약·촉매·용매 2

HCID 1140Toluene용매HCID 7967Cyclohexanone용매

실험 절차

A solution of 2.20 g cholesta-5,8-dien-3β-ol in 27 ml toluene and 6 ml cyclohexanone is refluxed for 10 minutes in a Dean-Stark apparatus. 0.57 g aluminum isopropoxide are added and the reaction mixture is refluxed for 30 minutes. After cooling and addition of sulfuric acid (2 N), the resulting mixture is extracted with ethyl acetate. The organic layer is separated, washed with saturated sodium bicarbonate solution and water, dried over anhydrous sodium sulphate and filtered. After evaporation of the solvent the residue is chromatographed with a mixture of hexane and ethyl acetate to give 1.53 g cholesta-4,8-dien-3-one as a white solid.

후처리

  1. temperaturethe reaction mixture is refluxed for 30 minutes
  2. temperatureAfter cooling
  3. extractionthe resulting mixture is extracted with ethyl acetate
  4. customThe organic layer is separated
  5. washwashed with saturated sodium bicarbonate solution and water
  6. dry with materialdried over anhydrous sodium sulphate
  7. filtrationfiltered
  8. customAfter evaporation of the solvent the residue
  9. customis chromatographed with a mixture of hexane and ethyl acetate

출처 및 근거

ORD 기록
ord-d60d95de93c94bd0a509a4c790034f67
출처 데이터셋
uspto-grants-2002_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06407086B2

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