Sodium Bicarbonate → HCID 13231125、化合物

HRID 905029ノート

反応式

HRID 905029 の反応式
[C:1]([CH2:9][CH2:10][CH2:11][CH2:12]Br)(=[O:8])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[CH2:14]([O:16][C:17]([NH:19][N:20]1[CH2:25][CH2:24][NH:23][CH2:22][CH2:21]1)=[O:18])[CH3:15].C(=O)([O-])O.[Na+]>C(O)C>[C:1]([CH2:9][CH2:10][CH2:11][CH2:12][N:23]1[CH2:22][CH2:21][N:20]([NH:19][C:17]([O:16][CH2:14][CH3:15])=[O:18])[CH2:25][CH2:24]1)(=[O:8])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1

参加物

5

反応物 3

HCID 516892Sodium BicarbonateHCID 111840715-bromo-1-phenyl-1-pentanoneHCID 13200156Ethyl piperazin-1-ylcarbamate

生成物 1

HCID 13231125HCID 13231125、化合物収率 91%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

17.0 g of 1-benzoyl-4-bromobutane, 13.4 g of 1-(ethoxycarbonylamino)piperazine and 17.8 g of sodium hydrogen carbonate were heated under reflux in ethanol for 6 hours with stirring. The insoluble materials were removed from the reaction mixture by filtration. The solvent was distilled off, and water was added to the residue. The mixture was extracted with benzene. The extract was recrystallized from benzene-hexane to give 21.4 g of 4-(4-benzoylbutyl)-1-(ethoxycarbonylamino)-piperazine having a melting point of 105° to 106° C.

後処理

  1. customThe insoluble materials were removed from the reaction mixture by filtration
  2. distillationThe solvent was distilled off
  3. additionwater was added to the residue
  4. extractionThe mixture was extracted with benzene
  5. customThe extract was recrystallized from benzene-hexane

出典と根拠

ORDレコード
ord-6ade663aa5af422791a2999fdf531c7d
出典データセット
uspto-grants-1983_12
特許番号
US04421754

反応ノート

読み込み中…