反应详情

温度

85 °C

A mixture of the product of step (i) (272 g, 0.93 mol), K2CO3 (256 g, 1.86 mol), methoxypropylamine (199 g, 2.22 mol) in MeCN (1.5 L) was stirred at 80-90° C. under N2 atmosphere for 16 hour. The reaction mixture was cooled to room temperature and filtered. The filtrate was concentrated to remove MeCN. MTBE (1 L) and H2O (1 L) were charged to the resulting mixture and washed with aqueous 1N—HCl (1 L). The aqueous phase was collected and basified by aqueous 2.5N—NaOH to pH=9-10, to afford the subtitle compound (ii) in solution, which was used for next step directly.

1. temperatureThe reaction mixture was cooled to room temperature
2. filtrationfiltered
3. concentrationThe filtrate was concentrated
4. customto remove MeCN
5. additionMTBE (1 L) and H2O (1 L) were charged to the resulting mixture
6. washwashed with aqueous 1N—HCl (1 L)
7. customThe aqueous phase was collected