Sodium Carbonate → 4-(3,4-Dichlorophenyl)-1-piperazinepentanenitrile

HRID 1871255

반응식

HRID 1871255 반응식
[Cl:1][C:2]1[CH:3]=[C:4]([N:9]2[CH2:14][CH2:13][NH:12][CH2:11][CH2:10]2)[CH:5]=[CH:6][C:7]=1[Cl:8].Cl[CH2:16][CH2:17][CH2:18][CH2:19][C:20]#[N:21].C(=O)([O-])[O-].[Na+].[Na+]>CC(C)CC(=O)C.[I-].[K+]>[Cl:1][C:2]1[CH:3]=[C:4]([N:9]2[CH2:14][CH2:13][N:12]([CH2:16][CH2:17][CH2:18][CH2:19][C:20]#[N:21])[CH2:11][CH2:10]2)[CH:5]=[CH:6][C:7]=1[Cl:8]

참가 물질

6

반응물 3

HCID 10340Sodium CarbonateHCID 804745-ChlorovaleronitrileHCID 936011-(3,4-Dichlorophenyl)piperazine

생성물 1

HCID 219996984-(3,4-Dichlorophenyl)-1-piperazinepentanenitrile수율 72.1%

시약·촉매·용매 2

HCID 4875Potassium Iodide촉매HCID 7909Methyl Isobutyl Ketone용매

실험 절차

A mixture of 1-(3,4-dichlorophenyl)piperazine (0.1 mol), 5-chloropentanenitrile (0.13 mol), sodium carbonate (10 g) and potassium iodide (0.1 g) in 4-methyl-2-pentanone (280 ml) was stirred and refluxed for 10 hours. The reaction mixture was cooled, filtered and the filtrate was evaporated. The residue was purified by column chromatography over silica gel (eluent: CH2Cl2 /CH3OH 95/5). The pure fractions were collected and the solvent was evaporated, yielding 22.5 g (72%) of 4-(3,4-dichlorophenyl)-1-piperazinepentanenitrile (interm. 2).

후처리

  1. temperaturerefluxed for 10 hours
  2. temperatureThe reaction mixture was cooled
  3. filtrationfiltered
  4. customthe filtrate was evaporated
  5. customThe residue was purified by column chromatography over silica gel (eluent: CH2Cl2 /CH3OH 95/5)
  6. customThe pure fractions were collected
  7. customthe solvent was evaporated

출처 및 근거

ORD 기록
ord-291ac4da5fee4cedb4d5e4a202d56366
출처 데이터셋
uspto-grants-2000_08
특허 번호
US06103725

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