Hydrochloric Acid → R 1364 (Steroid)

HRID 1077201ノート

反応式

HRID 1077201 の反応式
[CH2:1]([C@:4]12[CH2:12][CH2:11][C@@H:10]3[C:13]4[CH2:14][CH:15]=[C:16]([O:21]C)[CH2:17][C:18]=4[CH2:19][CH2:20][C@H:9]3[C@@H:8]1[CH2:7][CH2:6][C@@:5]2([C:24]#[CH:25])[OH:23])[CH2:2][CH3:3].Cl.O.CO>CCOCC>[CH2:1]([C@:4]12[CH2:12][CH2:11][C@@H:10]3[C@@H:13]4[C:18]([CH2:19][CH2:20][C@H:9]3[C@@H:8]1[CH2:7][CH2:6][C@:5]2([C:24]#[CH:25])[OH:23])=[CH:17][C:16](=[O:21])[CH2:15][CH2:14]4)[CH2:2][CH3:3]

参加物

6

反応物 4

HCID 313Hydrochloric AcidHCID 887MethanolHCID 962Water2 回HCID 86733485HCID 86733485、化合物

生成物 1

HCID 73602799R 1364 (Steroid)収率 33.6%

試薬・触媒・溶媒 1

HCID 3283Diethyl Ether溶媒

実験手順

Shake 13β-n-propyl-3-methoxy-17β-ethynyl-gona-2,5(10)-dien-17 -ol (0.31 g.) with a solution prepared by mixing concentrated hydrochloric acid (0.81 cc.), water (0.54 cc.) and methanol (12.15 cc.), until the solid dissolves. After addition of water, work up with ether, purify by recrystallization from cyclohexane to obtain the title compound (0.1 g.), m.p. 149°-50.5°; ultraviolet absorption peak at 240 mμ (ε15,700); infrared absorption peaks at 2.99, 3.06, 6.04, 6.16 μ.

後処理

  1. dissolutionuntil the solid dissolves
  2. custompurify by recrystallization from cyclohexane

出典と根拠

ORDレコード
ord-38544423709142e38776a2862590a572
出典データセット
uspto-grants-1976_05
特許番号
US03959322

反応ノート

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