Toluene → HCID 86740367、化合物

HRID 464153ノート

反応式

HRID 464153 の反応式
C([C@@]12[C@@H:20]3[C@H:11]([C@H:12]4[C@@:16]([CH2:18][CH2:19]3)([CH3:17])[C:15](=[O:21])[CH2:14][CH2:13]4)[CH2:10][CH2:9]C1=CC(=O)CC2)C.[C:23]1(Cl)C(=O)C(Cl)=C(Cl)C(=O)[C:24]=1Cl.[C:35]1([CH3:41])[CH:40]=[CH:39][CH:38]=[CH:37][CH:36]=1>>[CH2:41]=[C:35]1[CH2:40][CH2:39][C@@:38]2([CH2:23][CH3:24])[C:37]([CH:9]=[CH:10][C@@H:11]3[C@@H:20]2[CH2:19][CH2:18][C@@:16]2([CH3:17])[C@H:12]3[CH2:13][CH2:14][C:15]2=[O:21])=[CH:36]1

参加物

4

反応物 3

HCID 1140TolueneHCID 8371ChloranilHCID 1859950110beta-Ethyl-estra-4-ene-3,17-dione

生成物 1

HCID 86740367HCID 86740367、化合物

実験手順

290 mg of 10β-ethyl-estra-4-ene-3,17-dione and 594 mg of chloranil are taken up in 15 ml of toluene. The mixture is refluxed for 20 hours in an atmosphere of nitrogen. The solvent is washed with several small portions of 5% sodium hydroxide and then with water. It is dried over anhydrous sodium sulfate for several hours. The solution is filtered and the solvent removed under vacuum. The amorphous solid obtained is triturated with ether, filtered and purified by chromatography over silica gel using a n-hexane-ethyl acetate solvent.

後処理

  1. temperatureThe mixture is refluxed for 20 hours in an atmosphere of nitrogen
  2. washThe solvent is washed with several small portions of 5% sodium hydroxide
  3. dry with materialIt is dried over anhydrous sodium sulfate for several hours
  4. filtrationThe solution is filtered
  5. customthe solvent removed under vacuum
  6. customThe amorphous solid obtained
  7. customis triturated with ether
  8. filtrationfiltered
  9. custompurified by chromatography over silica gel using a n-hexane-ethyl acetate solvent

出典と根拠

ORDレコード
ord-c5a9462c548345a4b9e29d8527ecbb80
出典データセット
uspto-grants-1985_10
特許番号
US04546098

反応ノート

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