27409-41-2 → 3-Oxocholestane

HRID 267245ノート

反応式

HRID 267245 の反応式
[OH:1][CH:2]1[CH2:26][CH2:25][C@@:24]2([CH3:27])[CH:4]([CH2:5][CH2:6][C@@H:7]3[C@@H:23]2[CH2:22][CH2:21][C@@:20]2([CH3:28])[C@H:8]3[CH2:9][CH2:10][C@@H:11]2[C@H:12]([CH3:19])[CH2:13][CH2:14][CH2:15][CH:16]([CH3:18])[CH3:17])[CH2:3]1>[Si]([O-])([O-])([O-])[O-].[Ag+].[Ag+].[Ag+].[Ag+].C(OCC)(=O)C>[CH3:18][CH:16]([CH2:15][CH2:14][CH2:13][C@H:12]([C@@H:11]1[C@:20]2([CH3:28])[C@H:8]([C@H:7]3[C@H:23]([CH2:22][CH2:21]2)[C@:24]2([CH3:27])[CH:4]([CH2:3][C:2](=[O:1])[CH2:26][CH2:25]2)[CH2:5][CH2:6]3)[CH2:9][CH2:10]1)[CH3:19])[CH3:17]

参加物

4

反応物 1

HCID 1099274827409-41-2

生成物 1

HCID 108835733-Oxocholestane

試薬・触媒・溶媒 2

HCID 86733097HCID 86733097、化合物触媒2 回HCID 8857Ethyl Acetate溶媒

実験手順

388.6 Mg of 3-hydroxy-cholestane, 500 mg of silver silicate and 30 ml of ethyl acetate were added to the flask of Example II and the reaction mixture was refluxed for 10 hours. Another 50 mg of silver silicate were added thereto and reflux was continued for 5 hours. The mixture was then filtered and the filtrate was concentrated to dryness. The residue was dissolved in ether and the ether was distilled off under reduced pressure to obtain 383 mg of cholestane-3-one melting at 115°C, then 128°C.

後処理

  1. temperaturethe reaction mixture was refluxed for 10 hours
  2. temperaturereflux
  3. filtrationThe mixture was then filtered
  4. concentrationthe filtrate was concentrated to dryness
  5. dissolutionThe residue was dissolved in ether
  6. distillationthe ether was distilled off under reduced pressure

出典と根拠

ORDレコード
ord-4fbb10febead4223a6e2c96361c6023a
出典データセット
uspto-grants-1976_03
特許番号
US03941811

反応ノート

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