Sodium Stearate → 16beta-Ethyl-17beta-stearoyloxyacetoxy-4-estren-3-one

HRID 64716

反応式

HRID 64716 の反応式
[CH2:1]([C@H:3]1[CH2:8][C@H:7]2[C@H:9]3[C@H:18]([CH2:19][CH2:20][C@:5]2([CH3:6])[C@H:4]1[O:22][C:23](=[O:26])[CH2:24]Br)[C@@H:17]1[C:12](=[CH:13][C:14](=[O:21])[CH2:15][CH2:16]1)[CH2:11][CH2:10]3)[CH3:2].[C:27]([O-:46])(=[O:45])[CH2:28][CH2:29][CH2:30][CH2:31][CH2:32][CH2:33][CH2:34][CH2:35][CH2:36][CH2:37][CH2:38][CH2:39][CH2:40][CH2:41][CH2:42][CH2:43][CH3:44].[Na+]>CC(C)=O.O>[CH2:1]([C@H:3]1[CH2:8][C@H:7]2[C@H:9]3[C@H:18]([CH2:19][CH2:20][C@:5]2([CH3:6])[C@H:4]1[O:22][C:23](=[O:26])[CH2:24][O:46][C:27](=[O:45])[CH2:28][CH2:29][CH2:30][CH2:31][CH2:32][CH2:33][CH2:34][CH2:35][CH2:36][CH2:37][CH2:38][CH2:39][CH2:40][CH2:41][CH2:42][CH2:43][CH3:44])[C@@H:17]1[C:12](=[CH:13][C:14](=[O:21])[CH2:15][CH2:16]1)[CH2:11][CH2:10]3)[CH3:2]

参加物

4

反応物 2

HCID 2724691Sodium StearateHCID 1559376416beta-Ethyl-17beta-bromoacetoxy-4-estren-3-one

生成物 1

HCID 7046745016beta-Ethyl-17beta-stearoyloxyacetoxy-4-estren-3-one収率 57.1%

試薬・触媒・溶媒 1

HCID 18366337Propan-2-one--water (1/1)溶媒

実験手順

To 150 ml of acetone-water (2:1) are added 1.3 g of 16β-ethyl-17β-bromoacetoxy-4-estren-3-one and 1.0 g of sodium stearate and the mixture is refluxed for 4 hours and allowed to stand at room temperature (15°-25° C.) overnight. The solvent is then distilled off under reduced pressure and the residue is extracted with 150 ml of ethyl acetate. The organic layer is separated, washed with water and saturated aqueous sodium chloride and dried over anhydrous sodium sulfate. The solvent is distilled off under reduced pressure and the residue is dissolved in 100 ml of ethanol. To the solution is added 0.3 g of activated carbon and the insoluble material is filtered off. The solvent is distilled off to give a colorless viscous oil, which is allowed to stand at room temperature (15°-25° C.) to give 1.1 g of the above-identified compound as a solid.

後処理

  1. temperaturethe mixture is refluxed for 4 hours
  2. customto stand at room temperature
  3. custom(15°-25° C.) overnight
  4. distillationThe solvent is then distilled off under reduced pressure
  5. extractionthe residue is extracted with 150 ml of ethyl acetate
  6. customThe organic layer is separated
  7. washwashed with water and saturated aqueous sodium chloride
  8. dry with materialdried over anhydrous sodium sulfate
  9. distillationThe solvent is distilled off under reduced pressure
  10. dissolutionthe residue is dissolved in 100 ml of ethanol
  11. additionTo the solution is added 0.3 g of activated carbon
  12. filtrationthe insoluble material is filtered off
  13. distillationThe solvent is distilled off
  14. customto give a colorless viscous oil, which
  15. customto stand at room temperature
  16. custom(15°-25° C.)

出典と根拠

ORDレコード
ord-0682f4085c25476da26e2c16fc402b56
出典データセット
uspto-grants-1986_09
特許番号
US04609650

関連ノート

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