Piperidine → 4-Piperidin-1-ylbenzonitrile

HRID 1505167노트

반응식

Cl[C:2]1[CH:9]=[CH:8][C:5]([C:6]#[N:7])=[CH:4][CH:3]=1.[NH:10]1[CH2:15][CH2:14][CH2:13][CH2:12][CH2:11]1>>[N:10]1([C:2]2[CH:9]=[CH:8][C:5]([C:6]#[N:7])=[CH:4][CH:3]=2)[CH2:15][CH2:14][CH2:13][CH2:12][CH2:11]1

참가 물질

반응물 2

HCID 8082Piperidine

HCID 121634-Chlorobenzonitrile

생성물 1

HCID 7667714-Piperidin-1-ylbenzonitrile수율 89%

반응 조건

온도: 100 °C

실험 절차

To commercially available 4-chlorobenzonitrile 17 (1 g, 7.26 mmol) 3 ml of piperidine were added and the reaction was heated at 100° C. for 72 hours in closed vessel. The reaction was evaporated and the residue was dissolved in AcOEt and washed with water and brine. The purification of the crude residue by chromatographic column using AcOEt 1/Petroleum ether 9 as eluant gave 1.2 g of a pale yellow oil. Yield=89% 1HNMR (DMSO, 200 MHz) δ 1.57 (6H, m), 3.34 (4H, m), 6.98 (2H, d, J=9 Hz), 7.53 (2H, d, J=9 Hz)

후처리

customThe reaction was evaporated
dissolutionthe residue was dissolved in AcOEt
washwashed with water and brine
customThe purification of the crude residue by chromatographic column

출처 및 근거

ORD 기록: ord-1e0c9dab523544ef9e18f4b8b5dc5e5c
출처 데이터셋: uspto-grants-2015_12
DOI: 10.6084/m9.figshare.5104873.v1
특허 번호: US09216975B2

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