Hydrochloric Acid → Levonorgestrel

HRID 1077202

反応式

HRID 1077202 の反応式
[CH2:1]([C@:3]12[CH2:11][CH2:10][C@@H:9]3[C:12]4[CH2:13][CH2:14][C:15](=[O:20])[CH2:16][C:17]=4[CH2:18][CH2:19][C@H:8]3[C@@H:7]1[CH2:6][CH2:5][C@:4]2([C:22]#[CH:23])[OH:21])[CH3:2].CO.Cl>O>[CH2:1]([C@:3]12[CH2:11][CH2:10][C@@H:9]3[C@@H:12]4[C:17]([CH2:18][CH2:19][C@H:8]3[C@@H:7]1[CH2:6][CH2:5][C@:4]2([C:22]#[CH:23])[OH:21])=[CH:16][C:15](=[O:20])[CH2:14][CH2:13]4)[CH3:2]

参加物

5

反応物 3

HCID 313Hydrochloric AcidHCID 887MethanolHCID 29979902Levonorgestrel EP Impurity B

生成物 1

HCID 13109Levonorgestrel

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

Stir 13β-ethyl-17α-ethynyl-17β-hydroxy-gon-5(10)-en-3-one (0.1 g.) with a mixture of methanol (36 cc.), water (1.6 cc.) and concentrated hydrochloric acid (2.4 cc.) for 1 hour. Add water and extract the mixture with ether. Wash, dry and evaporate the ethereal solution and recrystallize the residue from ether-hexane to obtain the title compound, m.p. 203°-6° undepressed on admixture with authentic material. Infrared spectrum 3.05, 3.5, 6.05, 9.4 μ.

後処理

  1. extractionAdd water and extract the mixture with ether
  2. washWash
  3. customdry
  4. customevaporate the ethereal solution
  5. customrecrystallize the residue from ether-hexane

出典と根拠

ORDレコード
ord-b6289b2355f1482bbbfac433e467e2da
出典データセット
uspto-grants-1976_05
特許番号
US03959322

関連ノート

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