Methyl iodide → HCID 67359394、化合物
反応式
[CH2:1]([NH:3][C:4]([N:6]1[CH2:10][CH:9]([CH2:11][CH3:12])[CH:8]=[N:7]1)=[S:5])[CH3:2].I[CH3:14]>CO>[CH3:14][S:5][C:4]([N:6]1[CH2:10][CH:9]([CH2:11][CH3:12])[CH:8]=[N:7]1)=[N:3][CH2:1][CH3:2]参加物
4
反応条件
- 温度
- 50 °C
実験手順
1.80 g (1 mol equiv.) 4-Ethyl-4,5-dihydro-pyrazole-1-carbothioic acid ethylamide was dissolved in 36 mL methanol; 6.1 mL (10 mol equiv.) iodomethane was added and the reaction mixture was heated at 50° C. for 4 hours. Volatiles were removed under reduced pressure, and the residue was taken up in DCM and extracted with 5% aqueous NaHCO3. The organic layer was washed twice with water, dried over Na2SO4, filtered and evaporated to dryness to yield 1.68 g (87%) 4,N-diethyl-4,5-dihydro-pyrazole-1-carboximidothioic acid methyl ester. 1H NMR (400 MHz, CDCl3) δ 0.98 (t, J=7.5 Hz, 3H), 1.16 (t, J=7.3 Hz, 3H), 1.45-1.70 (m, 2H), 2.45 (s, 3H), 2.97-3.07 (m, 1H), 3.44 (dd, J=11.0, 8.3 Hz, 1H), 3.51-3.58 (m, 2H), 3.83 (t, J=11.0 Hz, 1H), 6.81 (s, 1H).