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Water → HCID 15838157, 화합물

HRID 1595971
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HRID 1595971 반응식
[OH:1][CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][C@@H:7]1[CH2:24][C:23]2[C@H:18]([CH2:19][CH2:20][C:21](=[O:25])[CH:22]=2)[C@@H:17]2[C@@H:8]1[C@H:9]1[C@@:13]([CH2:15][CH2:16]2)([CH3:14])[C:12](=[O:26])[CH2:11][CH2:10]1.[C:27](OC(=O)C)(=[O:29])[CH3:28].O>N1C=CC=CC=1.C(OCC)C>[C:27]([O:1][CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][C@@H:7]1[CH2:24][C:23]2[C@H:18]([CH2:19][CH2:20][C:21](=[O:25])[CH:22]=2)[C@@H:17]2[C@@H:8]1[C@H:9]1[C@@:13]([CH2:15][CH2:16]2)([CH3:14])[C:12](=[O:26])[CH2:11][CH2:10]1)(=[O:29])[CH3:28]
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참가 물질

6

반응물 3

HCID 962WaterHCID 7918Acetic AnhydrideHCID 158381567a-(5-Hydroxypentyl)-estr-4-ene-3,17-dione

생성물 1

HCID 15838157HCID 15838157, 화합물

시약·촉매·용매 2

HCID 1049Pyridine용매HCID 3283Diethyl Ether용매

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온도
25 °C

실험 절차

A solution of 94 g of crude 7α-(5-hydroxypentyl)-estr-4-ene-3,17-dione in 620 ml of pyridine is slowly mixed with 310 ml of acetic anhydride and stirred for 2 hours at 25° C. Then, it is slowly mixed with 116 ml of water while being cooled with ice, diluted with 3 l of diethyl ether, and, after washing with sodium bicarbonate solution, the organic phase is dried and concentrated by evaporation. The residue is chromatographed on silica gel, and 84.4 g of 7α-(5-acetoxypentyl)-estr-4-ene-3,17-dione is obtained as an oil.

후처리

  1. temperaturewhile being cooled with ice
  2. washafter washing with sodium bicarbonate solution
  3. customthe organic phase is dried
  4. concentrationconcentrated by evaporation
  5. customThe residue is chromatographed on silica gel

출처 및 근거

ORD 기록
ord-62e91cc880d14e86b65fce2cd03f1c9c
출처 데이터셋
uspto-grants-2001_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06288051B1

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