Acetic Anhydride → HCID 86738324、化合物

HRID 2059303ノート

反応式

HRID 2059303 の反応式
[OH:1][C@H:2]1[CH2:7][CH2:6][C@H:5]2[C@H:8]3[C@H:17]([CH2:18][CH2:19][C@:3]12[CH3:4])[C@:16]1([CH2:20][C:21]#[CH:22])[C:11](=[CH:12][C:13](=[O:23])[CH2:14][CH2:15]1)[CH2:10][CH2:9]3.[C:24](OC(=O)C)(=[O:26])[CH3:25]>N1C=CC=CC=1>[C:24]([O:1][C@H:2]1[CH2:7][CH2:6][C@H:5]2[C@H:8]3[C@H:17]([CH2:18][CH2:19][C@:3]12[CH3:4])[C@:16]1([CH2:20][C:21]#[CH:22])[C:11](=[CH:12][C:13](=[O:23])[CH2:14][CH2:15]1)[CH2:10][CH2:9]3)(=[O:26])[CH3:25]

参加物

4

反応物 2

HCID 7918Acetic AnhydrideHCID 86738323HCID 86738323、化合物

生成物 1

HCID 86738324HCID 86738324、化合物

試薬・触媒・溶媒 1

HCID 1049Pyridine溶媒

実験手順

To a solution of 500 mg of 17β-hydroxy-10-(2-propynyl)estr-4-en-3-one in 4 ml of pyridine at 25° C. is added 4 ml of acetic anhydride and the mixture is allowed to stand at room temperature for 16 hours. It is then concentrated under reduced pressure, the residue is diluted with ether and the ether solution is washed with 1 N hydrochloric acid and with aqueous sodium bicarbonate and then dried and concentrated. The resultant residue is recrystallized from ethyl acetate-hexane to give 17β-acetoxy-10-(2-propynyl)estr-4-en-3-one. This compound has the following structural formula ##STR10##

後処理

  1. concentrationIt is then concentrated under reduced pressure
  2. additionthe residue is diluted with ether
  3. washthe ether solution is washed with 1 N hydrochloric acid and with aqueous sodium bicarbonate
  4. customdried
  5. concentrationconcentrated
  6. customThe resultant residue is recrystallized from ethyl acetate-hexane

出典と根拠

ORDレコード
ord-d464cc13a68645ad85b336cfb766da39
出典データセット
uspto-grants-1982_03
特許番号
US04322416

反応ノート

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