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Water → 3alpha-N-methyl-dihydronicotinoyloxy-5alpha-pregnan-20-one

HRID 2253819
ノート
印刷プレビュー

反応式

HRID 2253819 の反応式
[I-].[CH3:2][N:3]1[CH:33]=[CH:32][CH:31]=[C:5]([C:6]([O:8][C@@H:9]2[CH2:28][CH2:27][C@@:26]3([CH3:29])[C@@H:11]([CH2:12][CH2:13][C@@H:14]4[C@@H:25]3[CH2:24][CH2:23][C@@:22]3([CH3:30])[C@H:15]4[CH2:16][CH2:17][C@@H:18]3[C:19](=[O:21])[CH3:20])[CH2:10]2)=[O:7])[CH2:4]1.C(=O)(O)[O-].[Na+].S(S([O-])=O)([O-])=O.[Na+].[Na+].O>CO>[CH3:2][N:3]1[CH2:33][CH:32]=[CH:31][CH:5]([C:6]([O:8][C@@H:9]2[CH2:28][CH2:27][C@@:26]3([CH3:29])[C@@H:11]([CH2:12][CH2:13][C@@H:14]4[C@@H:25]3[CH2:24][CH2:23][C@@:22]3([CH3:30])[C@H:15]4[CH2:16][CH2:17][C@@H:18]3[C:19](=[O:21])[CH3:20])[CH2:10]2)=[O:7])[CH2:4]1
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 962WaterHCID 24489Sodium DithioniteHCID 516892Sodium BicarbonateHCID 1317180393alpha-N-methyl-nicotinoyloxy,5alpha-pregnan-20-one iodide

生成物 1

HCID 677106683alpha-N-methyl-dihydronicotinoyloxy-5alpha-pregnan-20-one

試薬・触媒・溶媒 1

HCID 887
Methanol
溶媒

反応条件

温度
0 °C

実験手順

To an ice cold solution of the 3α-N-methyl-nicotinoyloxy-5α-pregnan-20-one iodide salt (1.01 g, 562 g/m, 1.8 mmol) in 150 mL of aqueous methanol (100 ml methanol and 50 ml water, deaerated) was added sodium bicarbonate (620 mg, 84 g/m, 7.4 mmol) and sodium dithionite (1.3 g, 174 g/m, 7.4 mmol). This mixture was stirred at 0° C. for 1 h. The reaction mixture was poured into 500 mL of water and extracted several times with chloroform. The combined organic layers were washed with potassium carbonate and concentrated. The crude product was filtered through a bed of silica gel using hexane/ethyl acetate (5:1) elution. The product was recovered in the initial fractions to give 180 mg (439 g/m, 0.4 mmol, 22%).

後処理

  1. extractionextracted several times with chloroform
  2. washThe combined organic layers were washed with potassium carbonate
  3. concentrationconcentrated
  4. filtrationThe crude product was filtered through a bed of silica gel
  5. washhexane/ethyl acetate (5:1) elution
  6. customThe product was recovered in the initial fractions
  7. customto give 180 mg (439 g/m, 0.4 mmol, 22%)

出典と根拠

ORDレコード
ord-ee02f86a0d724b7c9990ebb3d758804e
出典データセット
uspto-grants-1993_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05232917

反応ノート

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