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Potassium Carbonate → Tert-butyl 4-(3-ethoxy-3-oxopropyl)piperazine-1-carboxylate

HRID 397693
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HRID 397693 반응식
[CH2:1]([O:3][C:4](=[O:8])[CH2:5][CH2:6]Br)[CH3:2].[C:9]([O:13][C:14]([N:16]1[CH2:21][CH2:20][NH:19][CH2:18][CH2:17]1)=[O:15])([CH3:12])([CH3:11])[CH3:10].C(=O)([O-])[O-].[K+].[K+]>C(#N)C>[CH2:1]([O:3][C:4](=[O:8])[CH2:5][CH2:6][N:19]1[CH2:18][CH2:17][N:16]([C:14]([O:13][C:9]([CH3:12])([CH3:11])[CH3:10])=[O:15])[CH2:21][CH2:20]1)[CH3:2]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 11430Potassium CarbonateHCID 68320Ethyl 3-bromopropionateHCID 143452tert-Butyl piperazine-1-carboxylate

생성물 1

HCID 23000690Tert-butyl 4-(3-ethoxy-3-oxopropyl)piperazine-1-carboxylate

시약·촉매·용매 1

HCID 6342Acetonitrile용매

실험 절차

Ethyl-3-bromoproprionate (1.67 ml) was added to a suspension of tert-butyl-1-piperazine carboxylate (2.43 g) and potassium carbonate (2.16 g) in acetonitrile (30 ml). The reaction mixture was stirred for 56 hrs at room temperature, after which time the solvent was removed under reduced pressure and the residue partitioned between dichloromethane and water. The organic layer was separated, dried over magnesium sulphate and the solvent removed under reduced pressure to afford tert-butyl 4-(3-ethoxy-3-oxopropyl)-1-piperazinecarboxylate (2.44 g) as an oil.

후처리

  1. customafter which time the solvent was removed under reduced pressure
  2. customthe residue partitioned between dichloromethane and water
  3. customThe organic layer was separated
  4. dry with materialdried over magnesium sulphate
  5. customthe solvent removed under reduced pressure

출처 및 근거

ORD 기록
ord-0608739503a34c73b49ff52851d65f54
출처 데이터셋
uspto-grants-2003_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06610707B1

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