反应详情

温度

80 °C

To a solution of 8-benzyl-2-bromo-N-methyl-N-(1-methylethyl)-6,7,8,9-tetrahydropyrazino[2,3-f][1,4]oxazepin-3-amine (122 mg) in toluene (2 mL) was added 1-chloroethyl chloroformate (0.040 mL), and the mixture was stirred at 80° C. for 2 hr. The reaction mixture was cooled to room temperature, and concentrated. To the obtained residue was added methanol (2 mL), and the mixture was stirred at 80° C. for 1 hr. The reaction mixture was cooled to room temperature, and concentrated. The obtained residue was purified by recrystallization (methanol-diisopropyl ether) to give the title compound (59 mg, 56%) as pale-yellow crystals.

1. temperatureThe reaction mixture was cooled to room temperature
2. concentrationconcentrated
3. additionTo the obtained residue was added methanol (2 mL)
4. stirringthe mixture was stirred at 80° C. for 1 hr
5. temperatureThe reaction mixture was cooled to room temperature
6. concentrationconcentrated
7. customThe obtained residue was purified by recrystallization (methanol-diisopropyl ether)