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Potassium Carbonate → 2-(4-Benzylpiperidino)-4'-ethylpropiophenone

HRID 2308760
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HRID 2308760 반응식
Br[CH:2]([CH3:13])[C:3]([C:5]1[CH:10]=[CH:9][C:8]([CH2:11][CH3:12])=[CH:7][CH:6]=1)=[O:4].[CH2:14]([CH:21]1[CH2:26][CH2:25][NH:24][CH2:23][CH2:22]1)[C:15]1[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=1.C(=O)([O-])[O-].[K+].[K+]>C(O)C>[CH2:14]([CH:21]1[CH2:26][CH2:25][N:24]([CH:2]([CH3:13])[C:3]([C:5]2[CH:10]=[CH:9][C:8]([CH2:11][CH3:12])=[CH:7][CH:6]=2)=[O:4])[CH2:23][CH2:22]1)[C:15]1[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=1
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참가 물질

5

반응물 3

HCID 11430Potassium CarbonateHCID 317384-BenzylpiperidineHCID 201874952-Bromo-4'-ethylpropiophenone

생성물 1

HCID 201874892-(4-Benzylpiperidino)-4'-ethylpropiophenone

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

A mixture of 17.2 g of 2-bromo-4'-ethylpropiophenone, 12.5 g of 4-benzylpiperidine and 9.9 g of potassium carbonate in 250 ml of dry ethanol is heated under reflux for 4 hours, with stirring. The inorganic product is filtered off and washed with ethanol and the alcohol phase is concentrated in vacuo. The oily residue is taken up in diethyl ether and the mixture is extracted twice with dilute hydrochloric acid. After it has been rendered clearly alkaline with sodium hydroxide, the acid aqueous phase is then extracted three times with ethyl acetate. The organic phases are combined, washed with water until the washings are neutral, dried and evaporated in vauco. This give 19.15 g of an oily residue.

후처리

  1. temperatureis heated
  2. temperatureunder reflux for 4 hours
  3. filtrationThe inorganic product is filtered off
  4. washwashed with ethanol
  5. concentrationthe alcohol phase is concentrated in vacuo
  6. extractionthe mixture is extracted twice with dilute hydrochloric acid
  7. extractionthe acid aqueous phase is then extracted three times with ethyl acetate
  8. washwashed with water until the washings
  9. customdried
  10. customevaporated in vauco

출처 및 근거

ORD 기록
ord-28e10ce533724c5f8a8e2e720c0f0f9b
출처 데이터셋
uspto-grants-1987_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04690931

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