Ethylene Glycol → HCID 70505977、化合物

HRID 2418138ノート

反応式

HRID 2418138 の反応式
[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]

参加物

8

反応物 4

HCID 174Ethylene GlycolHCID 6101p-Toluenesulfonic acidHCID 31214Ethyl orthoformateHCID 12834728HCID 12834728、化合物

生成物 1

HCID 70505977HCID 70505977、化合物

試薬・触媒・溶媒 3

HCID 1049Pyridine溶媒HCID 3283Diethyl Ether溶媒HCID 6344Dichloromethane溶媒

実験手順

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.

後処理

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

出典と根拠

ORDレコード
ord-c7188e6a637e4a558293a6a8770e4e7d
出典データセット
uspto-grants-1984_09
特許番号
US04472310

反応ノート

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