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

HRID 434698ノート

反応式

HRID 434698 の反応式
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

参加物

5

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 6386tert-Butanol溶媒

実験手順

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.

後処理

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

出典と根拠

ORDレコード
ord-0f26040b80254976847da16edf57f8f8
出典データセット
uspto-grants-1983_08
特許番号
US04399141

反応ノート

読み込み中…