Water → HCID 86746635, 화합물

HRID 1613970

반응식

HRID 1613970 반응식
O.[C:2]([O:5][CH2:6][CH:7]([N+:32]([O-])=[O:33])[C:8]1[C@:25]2([CH3:26])[C@H:11]([C@H:12]3[C@:22]([OH:27])([CH2:23][CH2:24]2)[C@:20]2([CH3:21])[C:15]([CH2:16][C:17]4(OCC[O:28]4)[CH2:18][CH2:19]2)=[CH:14][CH2:13]3)[CH2:10][CH:9]=1)(=[O:4])[CH3:3].[Cl-].[Na+]>CC(C)=O.[Cr](Cl)(Cl)=O.[Cl-].[Cr+2].[Cl-].[Zn]>[C:2]([O:5][CH2:6][C:7](=[N:32][OH:33])[C:8]1[C@:25]2([CH3:26])[C@H:11]([C@H:12]3[C@:22]([OH:27])([CH2:23][CH2:24]2)[C@:20]2([CH3:21])[C:15](=[CH:16][C:17](=[O:28])[CH2:18][CH2:19]2)[CH2:14][CH2:13]3)[CH2:10][CH:9]=1)(=[O:4])[CH3:3]

참가 물질

8

반응물 3

HCID 962WaterHCID 5234Sodium ChlorideHCID 57121005HCID 57121005, 화합물

생성물 1

HCID 86746635HCID 86746635, 화합물

시약·촉매·용매 4

HCID 23994Zinc촉매HCID 10197677chromium(II) dichloride촉매HCID 178526110HCID 178526110, 화합물촉매HCID 180Acetone용매

실험 절차

A filtered aqueous solution of chromous chloride, prepared from chromium (II) chloride (26.1 g), water (121.8 ml) concentrated hydrochloric acid (52.2 ml) and zinc powder (15.7 g) according to the method of J. R. Hanson and T. D. Organ; J. Chem. Soc.(C) 1970, 1182, was added under nitrogen to a stirred solution of 21-acetoxy-3,3-ethylenedioxy-20-nitropregna-5,16-dien-9α-ol (8.70 g as a mixture of 2 diastereomers) in acetone (1.3 1). After stirring for 45 seconds the reaction mixture was poured into an aqueous sodium chloride solution. The resulting layers were separated after which the aqueous layer was washed twice with diethyl ether (400 ml). The combined organic layers were washed once with aqueous sodium chloride solution (450 ml), dried and evaporated under reduced pressure to afford the title compound.

후처리

  1. customThe resulting layers were separated after which the aqueous layer
  2. washwas washed twice with diethyl ether (400 ml)
  3. washThe combined organic layers were washed once with aqueous sodium chloride solution (450 ml)
  4. customdried
  5. customevaporated under reduced pressure

출처 및 근거

ORD 기록
ord-a11b45a2e8524fbb9a9e15d107021bf3
출처 데이터셋
uspto-grants-1993_03
특허 번호
US05194602

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