Pyridine → 1alpha-Methyl-17beta,19-di(trimethylsiloxy)-5alpha-androstan-3-one

HRID 1834967ノート

反応式

HRID 1834967 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@H:11]([CH2:12][C:13](=[O:23])[CH2:14][C@@H:15]1[CH3:22])[CH2:10][CH2:9]3.[CH3:24][Si:25]([CH3:28])([CH3:27])Cl.N1C=CC=CC=1>C1C=CC=CC=1>[CH3:22][C@@H:15]1[C@@:16]2([CH2:17][O:18][Si:25]([CH3:28])([CH3:27])[CH3:24])[C@@H: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:25]([CH3:28])([CH3:27])[CH3:24])[CH2:12][C:13](=[O:23])[CH2:14]1

参加物

5

反応物 3

HCID 1049PyridineHCID 6397ChlorotrimethylsilaneHCID 7061509617beta,19-Dihydroxy-1alpha-methyl-5alpha-androstan-3-one

生成物 1

HCID 228015331alpha-Methyl-17beta,19-di(trimethylsiloxy)-5alpha-androstan-3-one

試薬・触媒・溶媒 1

HCID 241Benzene溶媒

実験手順

A mixture of 17β,19-dihydroxy-1α-methyl-5α-androstan-3-one, trimethylchlorosilane and pyridine in benzene is heated to its reflux temperature for a period of about 14 hours. The reaction mixture is vacuum filtered, the organic layer is washed with water, dried over magnesium sulfate and concentrated in vacuum. Crystallization of the residue from hexane yields 1α-methyl-17β,19-di(trimethylsiloxy)-5α-androstan-3-one.

後処理

  1. temperatureis heated to its
  2. temperaturereflux temperature for a period of about 14 hours
  3. filtrationfiltered
  4. washthe organic layer is washed with water
  5. dry with materialdried over magnesium sulfate
  6. concentrationconcentrated in vacuum
  7. customCrystallization of the residue from hexane

出典と根拠

ORDレコード
ord-c9260c3151d44116bb965af33edb6bef
出典データセット
uspto-grants-1978_01
特許番号
US04071625

反応ノート

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