홈MCP워크벤치Skills
홈워크벤치알림마이페이지
llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0
  1. 홈
  2. /반응

Diethyl Ether → 3,3-Ethylenedioxy-1alpha-methyl-5alpha-androstan-17-one

HRID 262966
노트
인쇄 미리보기

반응식

HRID 262966 반응식
[CH2:1]1[CH2:25][O:24][C:3]2([CH2:20][C@H:19]([CH3:21])[C@@:18]3([CH3:22])[C@@H:5]([CH2:6][CH2:7][C@@H:8]4[C@@H:17]3[CH2:16][CH2:15][C@@:13]3([CH3:14])[C@H:9]4[CH2:10][CH2:11][C@@H:12]3[OH:23])[CH2:4]2)[O:2]1.[Al].CCOCC>C1(C)C=CC=CC=1.C1(=O)CCCCC1>[CH2:25]1[CH2:1][O:2][C:3]2([CH2:20][C@H:19]([CH3:21])[C@@:18]3([CH3:22])[C@@H:5]([CH2:6][CH2:7][C@@H:8]4[C@@H:17]3[CH2:16][CH2:15][C@@:13]3([CH3:14])[C@H:9]4[CH2:10][CH2:11][C:12]3=[O:23])[CH2:4]2)[O:24]1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 3

HCID 3283Diethyl EtherHCID 5359268AluminumHCID 13020861HCID 13020861, 화합물

생성물 1

HCID 130208633,3-Ethylenedioxy-1alpha-methyl-5alpha-androstan-17-one수율 93.3%

시약·촉매·용매 2

HCID 1140Toluene용매2회HCID 7967
Cyclohexanone
용매

실험 절차

55 g of 3,3-ethylenedioxy-17β-hydroxy-1α-methyl-5α-androstane in 550 ml of toluene and 110 ml of cyclohexanone were treated at boiling with a solution of 5.5 g of aluminium isopropylate in 55 ml of toluene and the mixture was heated for 3 hours with slow distillation. The mixture was then treated with ether, washed with ice-cold dilute sulphuric acid and water, evaporated and the residue steam-distilled. After extraction with methylene chloride, the resulting product was recrystallised from diisopropyl ether to give 51 g of 3,3-ethylenedioxy-1α-methyl-5α-androstan-17-one of melting point 155.5°-156.6° C.

후처리

  1. temperaturethe mixture was heated for 3 hours with slow distillation
  2. washwashed with ice-cold dilute sulphuric acid and water
  3. customevaporated
  4. distillationthe residue steam-distilled
  5. extractionAfter extraction with methylene chloride
  6. customthe resulting product was recrystallised from diisopropyl ether

출처 및 근거

ORD 기록
ord-559e5ff3053b4fc98d557938fcdf9b1e
출처 데이터셋
uspto-grants-1979_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04155918

반응 노트

불러오는 중…

이 페이지에서참가 물질실험 절차후처리출처 및 근거반응 노트