1,4-Dibromobutane → Lesopitron

HRID 1735495노트

반응식

HRID 1735495 반응식
[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

참가 물질

6

반응물 4

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

생성물 1

HCID 60813Lesopitron

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-a8049e01f1284a618ec5125c334fa334
출처 데이터셋
uspto-grants-1996_07
특허 번호
US05536836

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