反应详情

温度

50 °C

3-Chloro-3-methyl-2-nitroso-1-(4-methyl-2-nitro-1H-imidazol-1-yl) butane (3.41 g, 13.09 mmol) was added in portions to a stirred solution of N-(3-aminopropyl)-1-amino-1,1-dimethyl-2-butanone oxime (2.0 g, 11.56 mmol, Example 1) and (i-Pr)2NEt (1.64 g, 13.09 mmol) in dry acetonitrile (20 mL) at 50° C. under a nitrogen atmosphere. After the addition the reaction mixture was stirred for an additional 2 hours at 50° C. and cooled to room temperature. The solid which formed was filtered and recrystallized from acetonitrile to provide the title product as a light yellow colored solid. Yield: 3.08 g (59.4%); mp. 140-141° C.; 1H NMR (DMSO-d6) δ 1.12 & 1.19[2s, 6H, C(CH3)2], 1.33(m, 2H, CH2CH2CH2), 1.70[s, 3H, C(=N)CH3], 1.79 (bs, 2H, NH) 2.15(s, 3H, imi-CH3), 2.19(m, 4H, NHCH2), 5.19[s, 2H, NCH2C(=N)], 7.05 (s, 1H, imi-CH) and 10.33 & 11.36 (2s, 2H, NOH). MS m/e 398 (M+H)+.

1. additionAfter the addition the reaction mixture
2. temperaturecooled to room temperature
3. customThe solid which formed
4. filtrationwas filtered
5. customrecrystallized from acetonitrile