Pyridine → 1alpha-Methyl-17beta-trimethylsiloxy-4-androsten-19-one

HRID 2397981노트

반응식

HRID 2397981 반응식
[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([CH:17]=[O:18])[C:11](=[CH:12][CH2:13][CH2:14][C@@H:15]1[CH3:22])[CH2:10][CH2:9]3.[CH3:23][Si:24]([CH3:27])([CH3:26])Cl.N1C=CC=CC=1>C1C=CC=CC=1>[CH3:22][C@@H:15]1[C@@:16]2([CH:17]=[O:18])[C:11]([CH2:10][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[O:1][Si:24]([CH3:27])([CH3:26])[CH3:23])=[CH:12][CH2:13][CH2:14]1

참가 물질

5

반응물 3

HCID 1049PyridineHCID 6397ChlorotrimethylsilaneHCID 8673473617beta-Hydroxy-1alpha-methyl-4-androsten-19-one

생성물 1

HCID 227974621alpha-Methyl-17beta-trimethylsiloxy-4-androsten-19-one

시약·촉매·용매 1

HCID 241Benzene용매

실험 절차

A mixture of 17β-hydroxy-1α-methyl-4-androsten-19-one, trimethylchlorosilane and pyridine is refluxed in benzene for a period of about 18 hours. The suspension is filtered and the benzene removed under vacuum. The resulting oil is eluted from a silica gel chromatograph with benzene and crystallized from hexane to yield 1α-methyl-17β-trimethylsiloxy-4-androsten-19-one.

후처리

  1. filtrationThe suspension is filtered
  2. customthe benzene removed under vacuum
  3. washThe resulting oil is eluted from a silica gel chromatograph with benzene
  4. customcrystallized from hexane

출처 및 근거

ORD 기록
ord-48c98a8e1e484003ad2460da471f252f
출처 데이터셋
uspto-grants-1977_05
특허 번호
US04022769

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