反应详情

温度

20 °C

20 g (39 mmol) of 5-methyl-pyridine-2-sulfonic acid [6-chloro-2-(2-cyano-pyridine-4-yl)-5-(2-methoxy-phenoxy)-pyrimidine-4-yl]-amide were suspended in 100 ml of N,N-dimethyl formamide and 7.6 ml (156 mmol) of hydrazine hydrate were added within 15 min. The reaction mixture was allowed to warm up slowly to 20° C. After 17.5 hr, at a temperature of 15° C., 250 ml of de-ionized water were added followed by slow addition of 10.5 ml acetic acid (until pH=5.4). The resulting suspension was stirred for 2 hr at 20° C. and then for additional 2 hr 0° C. The solid was filtered off under suction, firstly washed with 200 ml of de-ionized water and thereafter with 100 ml of t-butylmethylether. The residue was dried at 40° C., 2000 Pa for 18 hr. There were obtained 21.7 g (102% of theory) of 5-methyl-pyridine-2-sulfonic acid [6-chloro-2-[2-(hydrazino-imino-methyl)-pyridine-4-yl]-5-(2-methoxy-phenoxy)-pyrimidine-4-yl]-amide with a HPLC purity of 81.4% (w/w).

1. waitfor additional 2 hr 0° C
2. filtrationThe solid was filtered off under suction
3. washfirstly washed with 200 ml of de-ionized water
4. customThe residue was dried at 40° C.
5. wait2000 Pa for 18 hr