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HCID 86735464, 화합물 → HCID 86735465, 화합물

HRID 616340
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HRID 616340 반응식
[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
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참가 물질

3

반응물 1

HCID 86735464HCID 86735464, 화합물

생성물 1

HCID 86735465HCID 86735465, 화합물

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

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.

후처리

  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
  • 출처 및 근거

    ORD 기록
    ord-21c73b8191d64ff08969a1bfe28bd331
    출처 데이터셋
    uspto-grants-1978_02
    DOI
    10.6084/m9.figshare.5104873.v1
    특허 번호
    US04073899

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