Pyridine → HCID 68142511、化合物

HRID 1657497ノート

反応式

HRID 1657497 の反応式
[CH2:1]([N:3]([CH2:6][C:7]1[CH2:8][C@@H:9]2[C@@H:25]([C@:26]3([CH3:33])[C:31]=1[CH2:30][C@@H:29]([OH:32])[CH2:28][CH2:27]3)[CH2:24][CH2:23][C@@:22]1([CH3:34])[C@H:10]2[CH2:11][CH2:12][C@@H:13]1[C@H:14]([CH3:21])[CH2:15][CH2:16][CH2:17][CH:18]([CH3:20])[CH3:19])[CH2:4][CH3:5])[CH3:2].N1C=CC=CC=1.[C:41](Cl)(=[O:44])[CH2:42][CH3:43].C(=O)(O)[O-].[K+]>O>[CH2:4]([N:3]([CH2:6][C:7]1[CH2:8][C@@H:9]2[C@@H:25]([C@:26]3([CH3:33])[C:31]=1[CH2:30][C@@H:29]([O:32][C:41](=[O:44])[CH2:42][CH3:43])[CH2:28][CH2:27]3)[CH2:24][CH2:23][C@@:22]1([CH3:34])[C@H:10]2[CH2:11][CH2:12][C@@H:13]1[C@H:14]([CH3:21])[CH2:15][CH2:16][CH2:17][CH:18]([CH3:19])[CH3:20])[CH2:1][CH3:2])[CH3:5]

参加物

6

反応物 4

HCID 1049PyridineHCID 62324Propionyl chlorideHCID 191548(1R,3aS,3bS,7S,9aR,9bS,11aR)‐5‐[(Diethylamino)methyl]‐9a,11a‐dimethyl‐1‐[(2R)‐6‐ methylheptan‐2‐yl]‐ 1H,2H,3H,3aH,3bH,4H,6H,7H,8H,9H,9aH,9bH,10H,11H,11aH‐cyclopenta[a]phenanthren‐7‐olHCID 516893Potassium Bicarbonate

生成物 1

HCID 68142511HCID 68142511、化合物

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

To a solution of 10 parts of 6-(diethylaminomethyl)cholest-5-en-3β-ol in 40 parts of pyridine at 0° is added, slowly and with stirring, 5 parts of propionyl chloride. When the addition is complete, stirring is continued for 2 hours while the reaction mixture warms to room temperature, whereupon 100 parts of water and 100 parts of aqueous 5% potassium bicarbonate are consecutively mixed in. The oil which separates is extracted with hexane. The extract is washed with water, dried over anhydrous sodium sulfate, and stripped of solvent by vacuum distillation, affording 6-(diethylaminomethyl)-3β-(propionyloxy)cholest-5-ene as the residue.

後処理

  1. additionWhen the addition
  2. stirringstirring
  3. additionare consecutively mixed in
  4. extractionThe oil which separates is extracted with hexane
  5. washThe extract is washed with water
  6. dry with materialdried over anhydrous sodium sulfate
  7. distillationstripped of solvent by vacuum distillation

出典と根拠

ORDレコード
ord-400ce63836d14681b6213510c204913a
出典データセット
uspto-grants-1976_06
特許番号
US03960904

反応ノート

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