Potassium Carbonate → 2-(3-piperidinopropyl)-4-phenyl-1(2H)-isoquinolone

HRID 1074617ノート

反応式

HRID 1074617 の反応式
Cl[CH2:2][CH2:3][CH2:4][N:5]1[CH:14]=[C:13]([C:15]2[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=2)[C:12]2[C:7](=[CH:8][CH:9]=[CH:10][CH:11]=2)[C:6]1=[O:21].C(=O)([O-])[O-].[K+].[K+]>N1CCCCC1>[N:5]1([CH2:2][CH2:3][CH2:4][N:5]2[CH:14]=[C:13]([C:15]3[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=3)[C:12]3[C:7](=[CH:8][CH:9]=[CH:10][CH:11]=3)[C:6]2=[O:21])[CH2:14][CH2:13][CH2:12][CH2:7][CH2:6]1

参加物

4

反応物 2

HCID 11430Potassium CarbonateHCID 128129652-(3-chloropropyl)-4-phenyl-1(2H)-isoquinolone

生成物 1

HCID 131747412-(3-piperidinopropyl)-4-phenyl-1(2H)-isoquinolone収率 180%

試薬・触媒・溶媒 1

HCID 8082Piperidine溶媒

実験手順

Then, 14.9 g of 2-(3-chloropropyl)-4-phenyl-1(2H)-isoquinolone, 7 g of anhydrous potassium carbonate and 40 ml of piperidine were mixed and heated at reflux for 5 hours. Thereafter, any excess of piperidine was distilled off and the residue was dissolved in dichloromethane. The solution was washed with water, dried and the solvent was distilled off. The resulting crystals were recrystallized from a mixture of diethyl ether and petroleum ether to obtain 15.6 g of 2-(3-piperidinopropyl)-4-phenyl-1(2H)-isoquinolone having a melting point of 117.5° C. as colorless prisms.

後処理

  1. temperatureheated
  2. temperatureat reflux for 5 hours
  3. distillationThereafter, any excess of piperidine was distilled off
  4. dissolutionthe residue was dissolved in dichloromethane
  5. washThe solution was washed with water
  6. customdried
  7. distillationthe solvent was distilled off
  8. customThe resulting crystals were recrystallized from a mixture of diethyl ether and petroleum ether

出典と根拠

ORDレコード
ord-ca40588b2ee04409a36c6936f2d90ad6
出典データセット
uspto-grants-1983_07
特許番号
US04393210

反応ノート

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