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HCID 86736737、化合物 → HCID 22809505、化合物

HRID 1448017
ノート
印刷プレビュー

反応式

HRID 1448017 の反応式
C(O)(=O)C.C(O)(=O)C.[OH:9][C@@H:10]1[CH2:35][CH2:34][C@@:33]2([CH3:36])[C@H:12]([C@@H:13]([OH:38])[CH2:14][C@@H:15]3[C@@H:32]2[CH2:31][CH2:30][C@@:29]2([CH3:37])[C@H:16]3[CH2:17][CH2:18][C@@H:19]2[C@H:20]([CH3:28])[CH2:21][CH2:22][C:23](=[O:27])[CH:24]([CH3:26])[CH3:25])[CH2:11]1>[OH-].[K+].CO>[OH:9][C@@H:10]1[CH2:35][CH2:34][C@@:33]2([CH3:36])[C@H:12]([C@@H:13]([OH:38])[CH2:14][C@@H:15]3[C@@H:32]2[CH2:31][CH2:30][C@@:29]2([CH3:37])[C@H:16]3[CH2:17][CH2:18][C@@H:19]2[C@H:20]([CH3:28])[CH2:21][CH2:22][C:23](=[O:27])[CH:24]([CH3:26])[CH3:25])[CH2:11]1
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 1

HCID 86736737HCID 86736737、化合物

生成物 1

HCID 22809505HCID 22809505、化合物

試薬・触媒・溶媒 2

HCID 887Methanol溶媒HCID 14797Potassium Hydroxide溶媒

実験手順

3α,6α-Dihydroxy-5β-cholestan-24-one diacetate prepared in Example 2 was dissolved in a solution of potassium hydroxide (11 g) in methanol (200 ml), and the solution was stirred at room temperature for 3 hours. The reaction mixture was concentrated into about 50 ml in volume. Water was added to the concentrate and the separated oil was extracted with ethyl acetate. The ethyl acetate layer was washed with water, dried over magnesium sulfate and evaporated. The residue was chromatographed on silica gel to give 3 g of 3α,6α-dihydroxy-5β-cholestan-24-one having a melting point of 180°-181° C. after recrystallization from ethyl acetate.

後処理

  1. concentrationThe reaction mixture was concentrated into about 50 ml in volume
  2. additionWater was added to the
  3. concentrationconcentrate
  4. extractionthe separated oil was extracted with ethyl acetate
  5. washThe ethyl acetate layer was washed with water
  6. dry with materialdried over magnesium sulfate
  7. customevaporated
  8. customThe residue was chromatographed on silica gel

出典と根拠

ORDレコード
ord-2ac2f6f917c646f5a7e072037ae79f42
出典データセット
uspto-grants-1979_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04179452

反応ノート

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このページの内容参加物実験手順後処理出典と根拠反応ノート