Acrylonitrile → 3-[4-(2,6-Dimethylphenyl)piperazin-1-yl]propionitrile

HRID 1070701노트

반응식

HRID 1070701 반응식
[CH3:1][C:2]1[CH:7]=[CH:6][CH:5]=[C:4]([CH3:8])[C:3]=1[N:9]1[CH2:14][CH2:13][NH:12][CH2:11][CH2:10]1.[C:15](#[N:18])[CH:16]=[CH2:17]>CO>[CH3:8][C:4]1[CH:5]=[CH:6][CH:7]=[C:2]([CH3:1])[C:3]=1[N:9]1[CH2:10][CH2:11][N:12]([CH2:17][CH2:16][C:15]#[N:18])[CH2:13][CH2:14]1

참가 물질

4

반응물 2

HCID 7855AcrylonitrileHCID 705381-(2,6-Xylyl)piperazine

생성물 1

HCID 223975343-[4-(2,6-Dimethylphenyl)piperazin-1-yl]propionitrile수율 78.6%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

4-(2,6-Dimethylphenyl) piperazine (1 g, 5.23 mmol) in MeOH (10 ml) was cooled to 0° and 0.305 g (5.73 mmol) of acrilonitrile was added. The reaction was stirred overnight at room temperature and evaporated under vacuum affording 1 g of crude 3-[4-(2,6-dimethylphenyl)piperazin-1-yl]propionitrile as a waxy solid. This compound was dissolved in MeOH (60 ml), 2 ml 37% HCl and hydrogenated under pressure (40 psi) with 0.2 g of 10% Pd\C. The reaction was filtered and evaporated to dryness obtaining 1 g of the title compound, as a hydrochloride salt, that was used without further purification for the following reaction.

후처리

  1. customevaporated under vacuum

출처 및 근거

ORD 기록
ord-b9433cbfcbeb47489e0922af4d1aaeaa
출처 데이터셋
uspto-grants-2005_06
특허 번호
US06903117B2

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