反应详情

温度

130 °C

A mixture of 0.633 g (2.30 mmol) 7-methoxy-3-piperidin-4-yl-1,3,4,5-tetrahydro-1,3-benzodiazepin-2-one, 0.700 mg (2.28 mmol) (2-chloro-6-methoxypyridin-4-yl)-(5-fluoro-2,3-dihydroindol-1-yl)-methanone and 954 mg (6.90 mmol) potassium carbonate in 5.0 mL NMP was stirred for 8 h at 130° C. After cooling the reaction mixture to RT the precipitate formed was filtered off and purified by preparative HPLC. The fractions containing the product were combined and evaporated down i. vac. The residue obtained was digested in DMF and the product remaining as a solid was suction filtered and dried i. vac. The mother liquor was again purified by preparative HPLC, the fractions containing product were combined and evaporated down i. vac. The residue was triturated with ethanol, the solid product was suction filtered and dried i. vac.

1. temperatureAfter cooling the reaction mixture to RT the precipitate
2. customformed
3. filtrationwas filtered off
4. custompurified by preparative HPLC
5. additionThe fractions containing the product
6. customevaporated down i
7. customThe residue obtained
8. filtrationfiltered
9. customdried i
10. customThe mother liquor was again purified by preparative HPLC
11. additionthe fractions containing product
12. customevaporated down i
13. customThe residue was triturated with ethanol
14. filtrationfiltered
15. customdried i