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Estrone → HCID 53662925, 화합물

HRID 1576350
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HRID 1576350 반응식
[CH3:1][C@@:2]12[C:18](=[O:19])[CH2:17][CH2:16][C@H:15]1[C@H:14]1[C@@H:5]([C:6]3[CH:7]=[CH:8][C:9]([OH:20])=[CH:10][C:11]=3[CH2:12][CH2:13]1)[CH2:4][CH2:3]2.[C:21]1([CH2:27][C:28](Cl)=[O:29])[CH:26]=[CH:25][CH:24]=[CH:23][CH:22]=1>N1C=CC=CC=1.O>[C:21]1([CH2:27][C:28]([O:20][C:9]2[CH:8]=[CH:7][C:6]3[C@@H:5]4[C@H:14]([C@H:15]5[C@@:2]([CH2:3][CH2:4]4)([CH3:1])[C:18](=[O:19])[CH2:17][CH2:16]5)[CH2:13][CH2:12][C:11]=3[CH:10]=2)=[O:29])[CH:26]=[CH:25][CH:24]=[CH:23][CH:22]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 2

HCID 5870EstroneHCID 7679Phenylacetyl chloride

생성물 1

HCID 53662925HCID 53662925, 화합물

시약·촉매·용매 2

HCID 962Water용매HCID 1049Pyridine용매

실험 절차

Oestrone (2 g.) in pyridine (10 ml.) was treated for three days at room temperature with phenylacetyl chloride (3 ml.). The mixture was diluted with water (50 ml.) and the product extracted with ether (50 ml.) containing a little chloroform. The extract was washed with water (50 ml.) then 2N-sulphuric acid (25 ml.) then water again (50 ml.) and the solvent was evaporated in vacuo. Filtration of the residue in methylene chloride through a short Florisil column and crystallisation from light petroleum (b.p. 40°/60°)-ether gave the title compound in two crops (total 1.54 g., 54%), m.p. 114°-116°.

후처리

  1. extractionthe product extracted with ether (50 ml.)
  2. additioncontaining a little chloroform
  3. washThe extract was washed with water (50 ml.)
  4. custom2N-sulphuric acid (25 ml.) then water again (50 ml.) and the solvent was evaporated in vacuo
  5. filtrationFiltration of the residue in methylene chloride
  6. customthrough a short Florisil column and crystallisation from light petroleum (b.p. 40°/60°)-ether

출처 및 근거

ORD 기록
ord-169d2b2ef04346e5990ec84096af400e
출처 데이터셋
uspto-grants-1976_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US03980681

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