反应详情

6-[4-[(2-Methylpropan-2-yl)oxycarbonyl]piperazin-1-yl]pyridine-3-carboxylic acid (150 mg, 0.412 mmol) was dissolved in dry THF (10 ml), 1-chloro-N,N,2-trimethyl-prop-1-en-1-amine (65 μl, 0.412 mmol) was added and the mixture was stirred at room temperature under nitrogen overnight. Pyridine (40 μl, 0.412 mmol) and tert-butyl 5-amino-3-[(3,5-dimethoxyphenyl)methoxy]pyrazole-1-carboxylate (142 mg, 0.343 mmol) were added and the mixture was stirred at 65° C. for 18 h. The mixture was then cooled to room temperature and stirred overnight with 4 M HCl in dioxane (1.8 ml, 7.20 mmol). The mixture was then filtered and the solid was washed with hexane. The product was purified on acidic prep. HPLC, eluting with a gradient of 16-26% MeCN in water (containing 0.1% TFA). The product containing fractions were neutralised with aq. NaHCO3 and the acetonitrile removed under vacuum. The product precipitated out and was collected by filtration. This was further washed with water and dried in vacuo to give the title compound (39 mg, 26%) as a white

1. stirringthe mixture was stirred at 65° C. for 18 h
2. temperatureThe mixture was then cooled to room temperature
3. filtrationThe mixture was then filtered
4. washthe solid was washed with hexane
5. customThe product was purified on acidic prep
6. washHPLC, eluting with a gradient of 16-26% MeCN in water (containing 0.1% TFA)
7. additionThe product containing fractions
8. customthe acetonitrile removed under vacuum
9. customThe product precipitated out
10. filtrationwas collected by filtration
11. washThis was further washed with water
12. customdried in vacuo