Hydrochloric Acid → R 1364 (Steroid)

HRID 1077201노트

반응식

HRID 1077201 반응식
[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]

참가 물질

6

반응물 4

HCID 313Hydrochloric AcidHCID 887MethanolHCID 962Water2회HCID 86733485HCID 86733485, 화합물

생성물 1

HCID 73602799R 1364 (Steroid)수율 33.6%

시약·촉매·용매 1

HCID 3283Diethyl Ether용매

실험 절차

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.

후처리

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

출처 및 근거

ORD 기록
ord-38544423709142e38776a2862590a572
출처 데이터셋
uspto-grants-1976_05
특허 번호
US03959322

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