1,1-Dimethylhydrazine → [4-(Dimethyl-hydrazono)-piperidin-1-yl]-dimethyl-amine

반응식

[CH3:1][N:2]([CH3:10])[N:3]1[CH2:8][CH2:7][C:6](=O)[CH2:5][CH2:4]1.[CH3:11][N:12]([CH3:14])[NH2:13]>>[CH3:11][N:12]([CH3:14])[N:13]=[C:6]1[CH2:7][CH2:8][N:3]([N:2]([CH3:10])[CH3:1])[CH2:4][CH2:5]1

참가 물질

반응물 2

HCID 59761,1-Dimethylhydrazine

HCID 567377821-(Dimethylamino)-4-piperidinone

생성물 1

HCID 67227495[4-(Dimethyl-hydrazono)-piperidin-1-yl]-dimethyl-amine수율 93.9%

실험 절차

3.0 g 1-Dimethylamino-piperidin-4-one (prepared as described in Journal of Medicinal & Pharmaceutical Chemistry, 4, 423-36; 1961) is cooled to 0° C., and 3.8 g N,N-dimethylhydrazine is added at such a rate, that the internal temperature does not exceed 15° C. The mixture is stirred at ambient temperature for 3 hours. Then the excess of N,N-dimethylhydrazine is evaporated. Thus, 3.65 g [4-(Dimethyl-hydrazono)-piperidin-1-yl]-dimethyl-amine is obtained. 1H-NMR (CDCl3): 2.80 ppm (m, 2H), 2.70 ppm (m, 4H), 2.45 ppm (s, 6H), 2.42 ppm (m, 2H), 2.40 ppm (s, 6H).

후처리

customdoes not exceed 15° C
customThen the excess of N,N-dimethylhydrazine is evaporated

출처 및 근거

ORD 기록: ord-7d02794213254b14860cca0a61ad4295
출처 데이터셋: uspto-grants-2013_09
DOI: 10.6084/m9.figshare.5104873.v1
특허 번호: US08541343B2

반응 노트

불러오는 중…