Piperidine → 10-(1-Piperidinyl)-5H-dibenzo[a,d]cyclohepten-5-one

HRID 434698노트

반응식

HRID 434698 반응식
Br[C:2]1[C:8]2[CH:9]=[CH:10][CH:11]=[CH:12][C:7]=2[C:6](=[O:13])[C:5]2[CH:14]=[CH:15][CH:16]=[CH:17][C:4]=2[CH:3]=1.[NH:18]1[CH2:23][CH2:22][CH2:21][CH2:20][CH2:19]1.CC(C)([O-])C.[K+]>C(O)(C)(C)C>[N:18]1([C:2]2[C:8]3[CH:9]=[CH:10][CH:11]=[CH:12][C:7]=3[C:6](=[O:13])[C:5]3[CH:14]=[CH:15][CH:16]=[CH:17][C:4]=3[CH:3]=2)[CH2:23][CH2:22][CH2:21][CH2:20][CH2:19]1

참가 물질

5

반응물 3

HCID 8082PiperidineHCID 1243721510-Bromo-5H-dibenzo[a,d][7]annulen-5-oneHCID 23665647Potassium tert-butoxide

생성물 1

HCID 1109822610-(1-Piperidinyl)-5H-dibenzo[a,d]cyclohepten-5-one

시약·촉매·용매 1

HCID 6386tert-Butanol용매

실험 절차

A mixture of 71.3 g of 10-bromo-5H-dibenzo[a,d]cyclohepten-5-one, 50 ml. of piperidine, 1 liter of t-butanol and finally 33.6 g of potassium t-butoxide was stirred under reflux 2 hours, then at room temperature overnight. The mixture was filtered, and concentrated to dryness. The residue was slurried with water and decanted. The residue was slurried with methanol and filtered to give 59.8 g of 10-(1-piperidyl)-5H-dibenzo[a,d]cyclohepten-5-one, m.p. 103°-105° C.

후처리

  1. temperatureunder reflux 2 hours
  2. customat room temperature
  3. customovernight
  4. filtrationThe mixture was filtered
  5. concentrationconcentrated to dryness
  6. customdecanted
  7. filtrationfiltered

출처 및 근거

ORD 기록
ord-0f26040b80254976847da16edf57f8f8
출처 데이터셋
uspto-grants-1983_08
특허 번호
US04399141

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