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Ethylene Glycol → HCID 15086123, 화합물

HRID 1885559
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HRID 1885559 반응식
[C:1]([O:4][C:5]1[CH:22]=[CH:21][C:20]2[C@@H:19]3[C@H:10]([C@H:11]4[C@@:15]([CH2:17][CH2:18]3)([CH3:16])[C:14](=[O:23])[CH2:13][CH2:12]4)[C@H:9]([CH2:24][CH2:25][CH2:26][CH2:27][CH2:28][CH2:29][CH2:30][CH2:31][CH2:32][CH2:33][CH2:34][O:35][C:36](=[O:38])[CH3:37])[CH2:8][C:7]=2[CH:6]=1)(=[O:3])[CH3:2].[CH2:39](O)[CH2:40][OH:41].C(OC)(OC)OC.C1(C)C=CC(S(O)(=O)=O)=CC=1>ClCCl>[C:1]([O:4][C:5]1[CH:22]=[CH:21][C:20]2[C@@H:19]3[C@H:10]([C@H:11]4[C@@:15]([CH2:17][CH2:18]3)([CH3:16])[C:14]3([O:41][CH2:40][CH2:39][O:23]3)[CH2:13][CH2:12]4)[C@H:9]([CH2:24][CH2:25][CH2:26][CH2:27][CH2:28][CH2:29][CH2:30][CH2:31][CH2:32][CH2:33][CH2:34][O:35][C:36](=[O:38])[CH3:37])[CH2:8][C:7]=2[CH:6]=1)(=[O:3])[CH3:2]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 174Ethylene GlycolHCID 6101p-Toluenesulfonic acidHCID 9005Trimethyl orthoformateHCID 150861223-Acetoxy-7alpha-(11-acetoxyundecyl)-1,3,5(10)-estratrien-17-one

생성물 1

HCID 15086123HCID 15086123, 화합물

시약·촉매·용매 1

HCID 6344
Dichloromethane
용매
2회

실험 절차

7.85 g of 3-acetoxy-7α-(11-acetoxyundecyl)-1,3,5(10)-estratrien-17-one is stirred under reflux in 51 ml of dichloromethane and 51 ml of ethylene glycol with 24 ml of trimethyl orthoformate and 159 mg of p-toluenesulfonic acid for 0.5 hour. For working up purposes, the mixture is diluted with dichloromethane, washed with sodium bicarbonate and sodium chloride solutions, dried over sodium sulfate, concentrated to dryness under vacuum, and chromatographed on silica gel with hexane/ethyl acetate, yielding 6.5 g of pure 3-acetoxy-7α-(11-acetoxyundecyl)-17,17-ethylenedioxy-1,3,5(10)-estratriene, [α]D =13.4°, as an oil.

후처리

  1. washwashed with sodium bicarbonate and sodium chloride solutions
  2. dry with materialdried over sodium sulfate
  3. concentrationconcentrated to dryness under vacuum
  4. customchromatographed on silica gel with hexane/ethyl acetate

출처 및 근거

ORD 기록
ord-e24f30135f1b4ec59ebadff5967b1a5f
출처 데이터셋
uspto-grants-1992_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05145847

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