Water → HCID 68560345、化合物

HRID 1876735ノート

反応式

HRID 1876735 の反応式
[OH:1][C@@H:2]1[C@H:7]2[C@H:8]3[C@H:18]([CH2:19][CH2:20][C@:5]2([CH3:6])[C:4](=O)[CH2:3]1)[C@:16]1([CH3:17])[C:11](=[CH:12][C:13](=[O:21])[CH2:14][CH2:15]1)[CH2:10][CH2:9]3.[C:23](OC(=O)C)(=[O:25])[CH3:24].[OH2:30]>O1CCCC1.CN(C)C1C=CN=CC=1>[C:23]([O:1][C@@H:2]1[C@H:7]2[C@H:8]3[C@H:18]([CH2:19][CH2:20][C@:5]2([CH3:6])[CH2:4][CH2:3]1)[C@:16]1([CH3:17])[C:11](=[CH:12][C:13](=[O:21])[CH2:14][CH2:15]1)[CH2:10][C:9]3=[O:30])(=[O:25])[CH3:24]

参加物

6

反応物 3

HCID 962WaterHCID 7918Acetic AnhydrideHCID 1165238315alpha-Hydroxyandrost-4-ene-3,17-dione

生成物 1

HCID 68560345HCID 68560345、化合物収率 88%

試薬・触媒・溶媒 2

HCID 142844-(Dimethylamino)pyridine触媒HCID 8028Tetrahydrofuran溶媒

実験手順

According to this invention the 15α-hydroxy-androst-4-ene-3,17-dione of the formula (III) preferably is reacted with acetic anhydride in dry tetrahydrofuran in the presence of 4-dimethylaminopyridine below a temperature of 40° C., after the reaction has been completed the reaction mixture is added to water, when the precipitate is dense enough it is filtered, washed until free of mother liquor and dried. The 15α-acetoxy-androst-4-ene-3,7-dione is obtained with 88% yield. The reaction is easy-to-carry out, there are no safety and scale-up problems. The 15α-acetoxy compound obtained can be used in the next reaction step without purification.

後処理

  1. filtrationis filtered
  2. washwashed until free of mother liquor
  3. customdried

出典と根拠

ORDレコード
ord-4fb3c416d0504fa7b196ed68e81c1f5e
出典データセット
uspto-grants-2012_11
特許番号
US08309712B2

反応ノート

読み込み中…