Sodium Bicarbonate → HCID 13231125, 화합물

HRID 905029노트

반응식

HRID 905029 반응식
[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

참가 물질

5

반응물 3

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

생성물 1

HCID 13231125HCID 13231125, 화합물수율 91%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-6ade663aa5af422791a2999fdf531c7d
출처 데이터셋
uspto-grants-1983_12
특허 번호
US04421754

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