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Potassium sodium tartarate → 1alpha-Methyl-5-androstene-3beta,17beta,19-triol

HRID 1390734
ノート
印刷プレビュー

反応式

HRID 1390734 の反応式
[OH:1][C@H:2]1[CH2:7][CH2:6][C@H:5]2[C@H:8]3[C@H:19]([CH2:20][CH2:21][C@:3]12[CH3:4])[C@:16]1([CH2:17][OH:18])[C:11]([CH2:12][C:13](=[O:23])[CH2:14][C@@H:15]1[CH3:22])=[CH:10][CH2:9]3.[H-].[Al+3].[Li+].[H-].[H-].[H-].C(C(C(C([O-])=O)O)O)([O-])=O.[K+].[Na+]>O1CCCC1>[CH3:22][C@@H:15]1[C@@:16]2([CH2:17][OH:18])[C:11](=[CH:10][CH2:9][C@@H:8]3[C@@H:19]2[CH2:20][CH2:21][C@@:3]2([CH3:4])[C@H:5]3[CH2:6][CH2:7][C@@H:2]2[OH:1])[CH2:12][C@@H:13]([OH:23])[CH2:14]1
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 9855836Potassium sodium tartarateHCID 21226445Aluminium lithium hydrideHCID 7060471217beta,19-Dihydroxy-1alpha-methyl-5-androsten-3-one

生成物 1

HCID 706054601alpha-Methyl-5-androstene-3beta,17beta,19-triol

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒2 回

実験手順

A solution of 17β,19-dihydroxy-1α-methyl-5-androsten-3-one in tetrahydrofuran is added to a suspension of lithium aluminum hydride in tetrahydrofuran. After stirring overnight at room temperature an aqueous solution of sodium potassium tartrate is added until a readily filtered granular precipitate forms. This precipitate is removed by filtration and washed well with ether. The filtrate and ether washings are combined, washed with water, dried over magnesium sulfate and concentrated under vacuum. Crystallization of the residue yields 1α-methyl-5-androstene-3β,17β,19-triol.

後処理

  1. additionis added until a readily filtered granular precipitate forms
  2. customThis precipitate is removed by filtration
  3. washwashed well with ether
  4. washwashed with water
  5. dry with materialdried over magnesium sulfate
  6. concentrationconcentrated under vacuum
  7. customCrystallization of the residue

出典と根拠

ORDレコード
ord-ff94e25111c54368b78269d5f6333f61
出典データセット
uspto-grants-1979_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04139617

反応ノート

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