Ethylene Glycol → HCID 70505977, 화합물

HRID 2418138노트

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HRID 2418138 반응식
[C:1]([O:4][C@H:5]1[CH2:22][CH2:21][C@@:20]2([CH3:23])[C:7](=[CH:8][CH2:9][C@@H:10]3[C@@H:19]2[CH2:18][CH2:17][C@@:15]2([CH3:16])[C@H:11]3[C@@H:12]3[CH2:25][C@@H:13]3[C:14]2=[O:24])[CH2:6]1)(=[O:3])[CH3:2].[CH2:26](O)[CH2:27][OH:28].C(OCC)(OCC)OCC.C1(C)C=CC(S(O)(=O)=O)=CC=1>C(Cl)Cl.CCOCC.N1C=CC=CC=1>[C:1]([O:4][C@H:5]1[CH2:22][CH2:21][C@@:20]2([CH3:23])[C:7](=[CH:8][CH2:9][C@@H:10]3[C@@H:19]2[CH2:18][CH2:17][C@@:15]2([CH3:16])[C@H:11]3[C@@H:12]3[CH2:25][C@@H:13]3[C:14]32[O:28][CH2:27][CH2:26][O:24]3)[CH2:6]1)(=[O:3])[CH3:2]

참가 물질

8

반응물 4

HCID 174Ethylene GlycolHCID 6101p-Toluenesulfonic acidHCID 31214Ethyl orthoformateHCID 12834728HCID 12834728, 화합물

생성물 1

HCID 70505977HCID 70505977, 화합물

시약·촉매·용매 3

HCID 1049Pyridine용매HCID 3283Diethyl Ether용매HCID 6344Dichloromethane용매

실험 절차

A solution of 105 g of 3β-acetoxy-15β,16β-methylene-5-androsten-17-one in 1.05 l of methylene chloride was combined with 315 ml of ethylene glycol, 210 ml of triethyl orthoformate, and 10.5 g of p-toluene-sulfonic acid and agitated for 1 hour at room temperature. The reaction solution was combined with 40 ml of pyridine and diluted with ether, then washed with water, dried, and evaporated. The residue was triturated with pentane and vacuum-filtered, thus producing 109 mg of 3β-acetoxy-17,17-ethylenedioxy-15β,16β-methylene-5-androstene, mp 177°-178.5° C.

후처리

  1. washwashed with water
  2. customdried
  3. customevaporated
  4. customThe residue was triturated with pentane
  5. filtrationvacuum-filtered

출처 및 근거

ORD 기록
ord-c7188e6a637e4a558293a6a8770e4e7d
출처 데이터셋
uspto-grants-1984_09
특허 번호
US04472310

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