反应详情

温度

65 °C

A microwave vial was charged with (S,Z)—N-(7-bromo-3-chloro-1-fluorospiro[chromeno[2,3-c]pyridine-5,4′-[1,3]oxazinan]-2′-ylidene)benzamide (2.0 g, 3.98 mmol), Pd(dba)2 (0.073 g, 0.080 mmol) and (2-biphenyl)dicyclohexylphosphine (0.067 g, 0.191 mmol), sealed and purged with N2 followed by the addition of THF (2 mL) and lithium bis(trimethylsilyl)amide, 1.0 m solution in tetrahydrofuran (8.75 ml, 8.75 mmol). The resulting mixture was heated at 65° C. for 17 h, quenched with saturated NH4Cl. The mixture was diluted with EtOAc, washed with water, brine, and dried over Na2SO4. The solution was concentrated and chromatographed on silica gel using 0-100% EtOAc/hexanes to afford a yellow oil as (S,Z)—N-(7-amino-3-chloro-1-fluorospiro[chromeno[2,3-c]pyridine-5,4′-[1,3]oxazinan]-2′-ylidene)benzamide.

1. customsealed
2. custompurged with N2
3. customquenched with saturated NH4Cl
4. additionThe mixture was diluted with EtOAc
5. washwashed with water, brine
6. dry with materialdried over Na2SO4
7. concentrationThe solution was concentrated
8. customchromatographed on silica gel using 0-100% EtOAc/hexanes