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HCID 86735464、化合物 → HCID 86735465、化合物

HRID 616340
ノート
印刷プレビュー

反応式

HRID 616340 の反応式
[C:1]([OH:4])(=[O:3])[CH3:2].[OH:5][C@H:6]1[CH2:11][CH2:10][C@H:9]2[C@H:12]3[C@H:21]([CH2:22][CH2:23][C@:7]12[CH3:8])[C@@H:20]1[C:15]([CH2:16][C:17](=[O:24])[CH2:18][CH2:19]1)=[CH:14][C@H:13]3[CH3:25]>O1CCCC1>[C:1]([OH:4])(=[O:3])[CH3:2].[CH3:25][C@@H:13]1[CH:14]=[C:15]2[C@H:20]([CH2:19][CH2:18][C@H:17]([OH:24])[CH2:16]2)[C@@H:21]2[C@@H:12]1[C@H:9]1[C@@:7]([CH2:23][CH2:22]2)([CH3:8])[C@@H:6]([OH:5])[CH2:11][CH2:10]1
参加物実験手順後処理出典と根拠反応ノート

参加物

3

反応物 1

HCID 86735464HCID 86735464、化合物

生成物 1

HCID 86735465HCID 86735465、化合物

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

A solution of 17β-hydroxy-7α-methyl-estr-5-en-3-one acetate dissolved in tetrahydrofuran is purged with nitrogen and slowly added to a suspension of lithium tertiarybutoxyaluminum hydride also purged with nitrogen. The mixture is stirred at room temperature for about 16 hours and excess hydride is destroyed by cautiously adding a solution of sodium potassium tartrate. The solid which forms is removed by filtration and the filtrate is extracted with methylene chloride. The combined methylene chloride extracts are washed with water, dried and concentrated under vacuum. Recrystalization of the residue from acetone-hexane yields the desired 7α-methyl-estr-5-ene-3β,17β-diol acetate.

後処理

  1. custom
is purged with nitrogen
  • additionslowly added to a suspension of lithium tertiarybutoxyaluminum hydride
  • customalso purged with nitrogen
  • customexcess hydride is destroyed
  • additionby cautiously adding a solution of sodium potassium tartrate
  • customThe solid which forms is removed by filtration
  • extractionthe filtrate is extracted with methylene chloride
  • washThe combined methylene chloride extracts are washed with water
  • customdried
  • concentrationconcentrated under vacuum
  • customRecrystalization of the residue from acetone-hexane
  • 出典と根拠

    ORDレコード
    ord-21c73b8191d64ff08969a1bfe28bd331
    出典データセット
    uspto-grants-1978_02
    DOI
    10.6084/m9.figshare.5104873.v1
    特許番号
    US04073899

    反応ノート

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