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HCID 86736737、化合物 → HCID 22809505、化合物

HRID 28087
ノート
印刷プレビュー

反応式

HRID 28087 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 purified by chromatography on silica gel. Elution with chloroform gave 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 purified by chromatography on silica gel
  9. washElution with chloroform

出典と根拠

ORDレコード
ord-e33d5b34aacb44f1a64e63b9cd3a6d1e
出典データセット
uspto-grants-1980_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04225524

反応ノート

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