Potassium Carbonate → HCID 20187499、化合物

HRID 2308753ノート

反応式

HRID 2308753 の反応式
Br[CH2:2][C:3]([C:5]1[CH:10]=[CH:9][C:8]([Cl:11])=[CH:7][CH:6]=1)=[O:4].[CH2:12]([CH:19]1[CH2:24][CH2:23][NH:22][CH2:21][CH2:20]1)[C:13]1[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=1.C(=O)([O-])[O-].[K+].[K+]>C(O)C>[CH2:12]([CH:19]1[CH2:24][CH2:23][N:22]([CH2:2][C:3]([C:5]2[CH:10]=[CH:9][C:8]([Cl:11])=[CH:7][CH:6]=2)=[O:4])[CH2:21][CH2:20]1)[C:13]1[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=1

参加物

5

反応物 3

HCID 11430Potassium CarbonateHCID 317384-BenzylpiperidineHCID 68303p-Chlorophenacyl bromide

生成物 1

HCID 20187499HCID 20187499、化合物

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

A mixture of 23.35 g (0.1 mol) of 2-bromo-4'-chloroacetophenone, 17.5 g (0.1 mol) of 4-benzylpiperidine and 13.8 g (0.1 mol) of potassium carbonate in 250 ml of anhydrous ethanol is heated under reflux for 3 hours and then left to stand overnight. The inorganic materials are filtered off and washed with ethanol and the filtrate is evaporated in vacuo. A brown oily residue remains, which is triturated with diethyl ether. A solid forms and is filtered off and then washed with diethyl ether. The filtrate is collected and the solid is triturated with a mixture of dilute sodium hydroxide solution and ethyl acetate. The organic phase is separated off, washed, dried and combined with the previously obtained diethyl ether filtrate. After evaporation of the mixture in vacuo, an oil remains, which crystallises on standing and is used as such.

後処理

  1. temperatureis heated
  2. temperatureunder reflux for 3 hours
  3. waitleft
  4. filtrationThe inorganic materials are filtered off
  5. washwashed with ethanol
  6. customthe filtrate is evaporated in vacuo
  7. customwhich is triturated with diethyl ether
  8. filtrationA solid forms and is filtered off
  9. washwashed with diethyl ether
  10. customThe filtrate is collected
  11. customthe solid is triturated with a mixture of dilute sodium hydroxide solution and ethyl acetate
  12. customThe organic phase is separated off
  13. washwashed
  14. customdried
  15. customAfter evaporation of the mixture in vacuo
  16. customwhich crystallises

出典と根拠

ORDレコード
ord-e7f8d96a85b948a3b811fdf41c802d1a
出典データセット
uspto-grants-1987_09
特許番号
US04690931

反応ノート

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