反应详情

温度

80 °C

A solution of hydroxylamine hydrochloride (737 mg, 10.6 mmol) in water (3.0 mL) and 1 N aq. NaOH (11 mL) is added to 1-(2-isopropylamino-6-methyl-pyrimidin-4-yl)-ethanone (1.71 g, 8.85 mmol). The solution is stirred at 80° C. for 2 h and MeOH is added to maintain homogeneity of the mixture. The mixture is cooled to rt and the precipitate that forms is collected, washed with water and dried in vacuo to give 1-(2-isopropylamino-6-methyl-pyrimidin-4-yl)-ethanone oxime (1.54 g) as a yellow solid; LC-MS: tR=0.72 min, [M+H]+=209.52; 1H NMR (D6-DMSO): δ 1.15 (d, J=6.5 Hz, 6H), 2.10 (s, 3H), 2.25 (s, 3H), 4.07 (m, 1H), 6.80 (s, 1H), 6.86 (d, J=7.5 Hz, 1H), 11.62 (s, 1H).

1. temperatureto maintain homogeneity of the mixture
2. temperatureThe mixture is cooled to rt
3. customthe precipitate that forms is collected
4. washwashed with water
5. customdried in vacuo