Cesium carbonate → 4-[2-(5-Chloro-2-fluorophenyl)-6,7-dihydrofuro[3,2-d]pyrimidin-4-ylamino]-nicotinic acid ethyl ester

온도

80 °C

To a solution of 4-chloro-2-(5-chloro-2-fluorophenyl)-6,7-dihydrofuro[3,2-d]-pyrimidine (320 mg, 1.13 mmol, 1 eq) in dioxane (5 ml) was added Pd(OAc)2 (13 mg, 0.06 mmol, 0.05 eq) followed by BINAP (53 mg, 0.08 mmol, 0.075 eq), 4-amino-nicotinic acid ethyl ester (206 mg, 1.24 mmol, 1.1 eq) and Cs2CO3 (478 mg, 1.46 mmol, 1.5 eq). The reaction mixture was heated to 80° C. for 15 h. The reaction mixture was cooled to r.t. and filtered through Celite® and the crude material was purified by flash column chromatography (0-5% MeOH in CHCl3) to afford 4-[2-(5-chloro-2-fluorophenyl)-6,7-dihydrofuro[3,2-d]pyrimidin-4-ylamino]-nicotinic acid ethyl ester (100 mg, 21%) as a white solid.

1. temperatureThe reaction mixture was cooled to r.t.
2. filtrationfiltered through Celite®
3. customthe crude material was purified by flash column chromatography (0-5% MeOH in CHCl3)

ORD 기록

ord-26daa7813e00494cb7e04425f9090396

출처 데이터셋

uspto-grants-2011_07

DOI

10.6084/m9.figshare.5104873.v1

특허 번호

US07977342B2