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

HRID 2199046ノート

反応式

HRID 2199046 の反応式
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

参加物

6

反応物 4

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

実験手順

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.

後処理

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

出典と根拠

ORDレコード
ord-613b4dba2a814f92b4367ed0edb4cfd4
出典データセット
uspto-grants-1982_11
特許番号
US04361565

反応ノート

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