Piperazine → N-[4-(1-Piperazinyl)butyl]-3,3-dimethylglutarimide

HRID 2199046

반응식

HRID 2199046 반응식
Br[CH2:2][CH2:3][CH2:4][CH2:5][N:6]1[C:11](=[O:12])[CH2:10][C:9]([CH3:14])([CH3:13])[CH2:8][C:7]1=[O:15].CC1(C)CC(=O)NC(=O)C1.[NH:26]1[CH2:31][CH2:30][NH:29][CH2:28][CH2:27]1.C([O-])([O-])=O.[K+].[K+]>C(#N)C>[N:26]1([CH2:2][CH2:3][CH2:4][CH2:5][N:6]2[C:11](=[O:12])[CH2:10][C:9]([CH3:14])([CH3:13])[CH2:8][C:7]2=[O:15])[CH2:31][CH2:30][NH:29][CH2:28][CH2:27]1

참가 물질

6

반응물 4

HCID 4837PiperazineHCID 11430Potassium CarbonateHCID 142924,4-Dimethylpiperidine-2,6-dioneHCID 136603351-(4-Bromobutyl)-4,4-dimethylpiperidine-2,6-dione

생성물 1

HCID 20516935N-[4-(1-Piperazinyl)butyl]-3,3-dimethylglutarimide수율 85%

시약·촉매·용매 1

HCID 6342Acetonitrile용매

실험 절차

A mixture of N-(4-bromobutyl)-3,3-dimethylglutarimide (20.0 g; 0.07 mole [prepared from 3,3-dimethylglutarimide using the method of Example 2]); piperazine (31.0 g; 0.36 mole); K2CO3 (29.8 g; 0.22 mole); and KI (0.1 g) was refluxed in 250 mL acetonitrile for 18 hr. The mixture was filtered, concentrated and the unreacted piperazine removed by vacuum sublimation. The residual material was distilled to yield 17.2 g (85%) product, b.p. 170°-178° C. at 0.01 mm.

후처리

  1. filtrationThe mixture was filtered
  2. concentrationconcentrated
  3. customthe unreacted piperazine removed by vacuum sublimation
  4. distillationThe residual material was distilled

출처 및 근거

ORD 기록
ord-613b4dba2a814f92b4367ed0edb4cfd4
출처 데이터셋
uspto-grants-1982_11
특허 번호
US04361565

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