1,4-Dibromobutane → Lesopitron

HRID 1735495ノート

反応式

HRID 1735495 の反応式
[N:1]1([C:7]2[N:12]=[CH:11][CH:10]=[CH:9][N:8]=2)[CH2:6][CH2:5][NH:4][CH2:3][CH2:2]1.Br[CH2:14][CH2:15][CH2:16][CH2:17]Br.C([O-])([O-])=O.[K+].[K+].[Cl:25][C:26]1[CH:27]=[N:28][NH:29][CH:30]=1>CN(C)C=O>[Cl:25][C:26]1[CH:27]=[N:28][N:29]([CH2:14][CH2:15][CH2:16][CH2:17][N:4]2[CH2:5][CH2:6][N:1]([C:7]3[N:8]=[CH:9][CH:10]=[CH:11][N:12]=3)[CH2:2][CH2:3]2)[CH:30]=1

参加物

6

反応物 4

HCID 80561,4-DibromobutaneHCID 11430Potassium CarbonateHCID 275241H-Pyrazole, 4-chloro-HCID 887471-(2-Pyrimidinyl)piperazine

生成物 1

HCID 60813Lesopitron

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

To a mixture of 2- (1-piperazinyl)pyrimidine (32.8 g; 0.2 mol), 1,4-dibromobutane (47.5 g; 0.22 mol) and K2CO3 (69 g; 0.5 tool) in 400 ml of dimethylformamide is added 4 -chloropyrazole (20.5 g; 0.2 mol), and the mixture is held at the reflux for 17 hours. The reaction mixture is filtered hot and evaporated to dryness. The residue is dissolved in HCl, washed with CHCl3, rendered alkaline with dilute NaOH and extracted in basic medium with CHCl3. The organic phase is then dried and subsequently evaporated to dryness, and 61 g (95%) of 2-{4-[4-(4-chloro-1-pyrazolyl)butyl]-1-piperazinyl}pyrimidine are obtained.

後処理

  1. temperaturereflux for 17 hours
  2. filtrationThe reaction mixture is filtered hot
  3. customevaporated to dryness
  4. dissolutionThe residue is dissolved in HCl
  5. washwashed with CHCl3
  6. extractionextracted in basic medium with CHCl3
  7. customThe organic phase is then dried
  8. customsubsequently evaporated to dryness, and 61 g (95%) of 2-{4-[4-(4-chloro-1-pyrazolyl)butyl]-1-piperazinyl}pyrimidine
  9. customare obtained

出典と根拠

ORDレコード
ord-a8049e01f1284a618ec5125c334fa334
出典データセット
uspto-grants-1996_07
特許番号
US05536836

反応ノート

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