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Formaldehyde → 17beta-Hydroxy-17alpha-methyl-4-(phenylthiomethyl)androsta-4,15-dien-3-one

HRID 274303
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HRID 274303 반응식
[OH:1][C@@:2]1([CH3:22])[CH:7]=[CH:6][C@H:5]2[C@H:8]3[C@H:18]([CH2:19][CH2:20][C@:3]12[CH3:4])[C@:16]1([CH3:17])[C:11](=[CH:12][C:13](=[O:21])[CH2:14][CH2:15]1)[CH2:10][CH2:9]3.[C:23]1([SH:29])[CH:28]=[CH:27][CH:26]=[CH:25][CH:24]=1.[CH2:30]=O>N(CCO)(CCO)CCO>[OH:1][C@@:2]1([CH3:22])[CH:7]=[CH:6][C@H:5]2[C@H:8]3[C@H:18]([CH2:19][CH2:20][C@:3]12[CH3:4])[C@:16]1([CH3:17])[C:11](=[C:12]([CH2:30][S:29][C:23]2[CH:28]=[CH:27][CH:26]=[CH:25][CH:24]=2)[C:13](=[O:21])[CH2:14][CH2:15]1)[CH2:10][CH2:9]3
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참가 물질

5

반응물 3

HCID 712Formaldehyde2회HCID 7969Thiophenol2회HCID 1567913617beta-Hydroxy-17alpha-methylandrosta-4,15-dien-3-one

생성물 1

HCID 1567914117beta-Hydroxy-17alpha-methyl-4-(phenylthiomethyl)androsta-4,15-dien-3-one

시약·촉매·용매 1

HCID 7618Triethanolamine용매

실험 절차

Under argon, 9.2 g of 17β-hydroxy-17α-methylandrosta-4,15-dien-3-one in 80 ml of triethanolamine is allowed to react at 110° C. with 2.1 ml of thiophenol and 2.1 ml of aqueous formaldehyde solution (37%). After 5 hours and another 18 hours, respectively 2.1 ml of thiophenol and 2.1 ml of formaldehyde solution are added. In total, the reaction mixture is stirred for 32 hours and subsequently introduced into ice/water. The precipitated product is suctioned off, washed with water, taken up in methylene chloride, dried, and concentrated under vacuum. After chromatographing the crude product on silica gel with a hexane-ethyl acetate gradient, 7.9 g of 17β-hydroxy-17α-methyl-4-(phenylthiomethyl)androsta-4,15-dien-3-one is obtained, mp 146.8° C. (from acetone/hexane).

후처리

  1. washwashed with water
  2. customdried
  3. concentrationconcentrated under vacuum

출처 및 근거

ORD 기록
ord-ff640dddd972414dbaa189aa2ba81f45
출처 데이터셋
uspto-grants-1995_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05389624

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