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Hydrogen Peroxide → HCID 22859494, 화합물

HRID 1440973
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HRID 1440973 반응식
[NH:1]([C:5]1[C:22](=[O:23])[CH:21]=[CH:20][C@@:19]2([CH3:24])[C:6]=1[CH:7]=[CH:8][C@@H:9]1[C@@H:18]2[CH2:17][CH2:16][C@@:14]2([CH3:15])[C@H:10]1[CH2:11][CH2:12][C:13]2=[O:25])[C:2]([CH3:4])=[O:3].[OH:26]O.[OH-].[Na+]>CO.C(Cl)Cl>[NH:1]([C:5]1[C:22](=[O:23])[C@@H:21]2[O:26][CH:20]2[C@@:19]2([CH3:24])[C:6]=1[CH:7]=[CH:8][C@@H:9]1[C@@H:18]2[CH2:17][CH2:16][C@@:14]2([CH3:15])[C@H:10]1[CH2:11][CH2:12][C:13]2=[O:25])[C:2]([CH3:4])=[O:3]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 3

HCID 784Hydrogen PeroxideHCID 14798Sodium HydroxideHCID 228594964-Acetamino-androsta-1,4,6-triene-3,17-dione

생성물 1

HCID 22859494HCID 22859494, 화합물수율 80%

시약·촉매·용매 2

HCID 887Methanol용매HCID 6344Dichloromethane
용매

실험 절차

To an ice cold solution of 4-acetamino-androsta-1,4,6-triene-3,17-dione (3.384 g, 10 mmol) in methanol (50 ml) and CH2Cl2 (25 ml) are added gradually 35% H2O2 (4.5 ml) and 2N NaOH (1 ml). The mixture was allowed to stand at 0°-5° C. for 5 days. Then ice water was added, the mixture concentrated under vacuum to a small volume and the precipitate filtered off. Thus almost pure title compound was obtained (1.99 g). From the mother liquor 1.020 g of starting product was recovered. Therefore the yield is about 80% considering the recovery.

후처리

  1. concentrationthe mixture concentrated under vacuum to a small volume
  2. filtrationthe precipitate filtered off

출처 및 근거

ORD 기록
ord-8ad97c5c976c4abcb353f5aa0e4627b9
출처 데이터셋
uspto-grants-1996_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05502044

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