Water → HCID 70505471、化合物

HRID 2418143ノート

反応式

HRID 2418143 の反応式
[OH:1][C@H:2]1[CH2:19][CH2:18][C@@:17]2([CH3:20])[C:4](=[CH:5][CH2:6][C@@H:7]3[C@@H:16]2[CH2:15][CH2:14][C@@:12]2([CH3:13])[C@H:8]3[C@@H:9]3[CH2:22][C@@H:10]3[C:11]2=[O:21])[CH2:3]1.[C:23](Cl)(=[O:30])[C:24]1[CH:29]=[CH:28][CH:27]=[CH:26][CH:25]=1.O>N1C=CC=CC=1.C(Cl)Cl>[C:23]([O:1][C@H:2]1[CH2:19][CH2:18][C@@:17]2([CH3:20])[C:4](=[CH:5][CH2:6][C@@H:7]3[C@@H:16]2[CH2:15][CH2:14][C@@:12]2([CH3:13])[C@H:8]3[C@@H:9]3[CH2:22][C@@H:10]3[C:11]2=[O:21])[CH2:3]1)(=[O:30])[C:24]1[CH:29]=[CH:28][CH:27]=[CH:26][CH:25]=1

参加物

6

反応物 3

HCID 962WaterHCID 7412Benzoyl chlorideHCID 1307594915,16-Dihydro-3-hydroxy-3'H-cycloprop[15,16]androsta-5,15-dien-17-one

生成物 1

HCID 70505471HCID 70505471、化合物

試薬・触媒・溶媒 2

HCID 1049Pyridine溶媒HCID 6344Dichloromethane溶媒

実験手順

A solution of 5.0 g of 3β-hydroxy-15β,16β-methylene-5-androsten-17-one in 50 ml of pyridine was combined under ice cooling with 5 ml of benzoyl chloride and then stirred for 17 hours at room temperature. After the addition of 10 ml of water, the mixture was stirred for another hour; then the reaction solution was diluted with methylene chloride and washed with sodium carbonate solution and water. After drying and evaporation, the residue was triturated with diisopropyl ether and vacuum-filtered, thus obtaining 6.4 g of 3β-benzoyloxy-15β,16β-methylene-5-androsten-17-one, mp 250°-258° C.

後処理

  1. stirringthe mixture was stirred for another hour
  2. washwashed with sodium carbonate solution and water
  3. customAfter drying
  4. customevaporation
  5. customthe residue was triturated with diisopropyl ether
  6. filtrationvacuum-filtered

出典と根拠

ORDレコード
ord-420ed9d9aef647808eb71a6a51a8fca1
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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