Potassium Carbonate → Ethyl 3-[4-(3,3-diphenyl-1-propyl)piperazin-1-yl]benzoate

HRID 1796735노트

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HRID 1796735 반응식
[N:1]1([C:7]2[CH:8]=[C:9]([CH:15]=[CH:16][CH:17]=2)[C:10]([O:12][CH2:13][CH3:14])=[O:11])[CH2:6][CH2:5][NH:4][CH2:3][CH2:2]1.C(=O)([O-])[O-].[K+].[K+].[C:24]1([CH:30]([C:34]2[CH:39]=[CH:38][CH:37]=[CH:36][CH:35]=2)[CH2:31][CH2:32]Br)[CH:29]=[CH:28][CH:27]=[CH:26][CH:25]=1>CN(C)C=O>[C:24]1([CH:30]([C:34]2[CH:35]=[CH:36][CH:37]=[CH:38][CH:39]=2)[CH2:31][CH2:32][N:4]2[CH2:3][CH2:2][N:1]([C:7]3[CH:8]=[C:9]([CH:15]=[CH:16][CH:17]=3)[C:10]([O:12][CH2:13][CH3:14])=[O:11])[CH2:6][CH2:5]2)[CH:29]=[CH:28][CH:27]=[CH:26][CH:25]=1

참가 물질

5

반응물 3

HCID 11430Potassium CarbonateHCID 883331,1'-(3-Bromopropylidene)bisbenzeneHCID 11506913Ethyl 3-(piperazin-1-yl)benzoate

생성물 1

HCID 22180549Ethyl 3-[4-(3,3-diphenyl-1-propyl)piperazin-1-yl]benzoate수율 71.3%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

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온도
70 °C

실험 절차

The compound (1.60 g) prepared in step (a) was dissolved in N,N-dimethylformamide (20 ml). Potassium carbonate (2.79 g) and 3,3-diphenylpropyl bromide (2.82 g) were added to the solution. The mixture was stirred at 70° C. for 8 hr. The reaction solution was extracted with ethyl acetate, followed by washing with water and saturated brine. The organic layer was dried over anhydrous magnesium sulfate, and the solvent was then removed by distillation under the reduced pressure. The residue was purified by column chromatography on silica gel (chloroform:ethyl acetate=5:1) to give 2.00 g (71.3%) of ethyl 3-[4-(3,3-diphenyl-1-propyl)piperazin-1-yl]benzoate.

후처리

  1. extractionThe reaction solution was extracted with ethyl acetate
  2. washby washing with water and saturated brine
  3. dry with materialThe organic layer was dried over anhydrous magnesium sulfate
  4. customthe solvent was then removed by distillation under the reduced pressure
  5. customThe residue was purified by column chromatography on silica gel (chloroform:ethyl acetate=5:1)

출처 및 근거

ORD 기록
ord-24558fe9d78f4a89b5a50b255ee93ef4
출처 데이터셋
uspto-grants-2006_04
특허 번호
US07030120B2

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