反应详情

A solution of Intermediate 285C (250 mg, 1.452 mmol) in pyridine (5 mL) was stirred at 120° C. for 16 h. The reaction mixture was then cooled to RT, quenched with a 1.5 N aq. solution of HCl at 0° C., and extracted with diethyl ether (2×50 mL). The combined organic layers were washed with brine, dried over Na2SO4 and evaporated to afford Intermediate 285D as a viscous liquid (170 mg, 91% yield). 1H NMR (400 MHz, DMSO-d6) δ ppm 2.90-3.02 (m, 1H), 1.84-1.95 (m, 4H), 1.07-1.14 (m, 3H), 0.99-1.07 (m, 3H).

1. customquenched with a 1.5 N aq. solution of HCl at 0° C.
2. extractionextracted with diethyl ether (2×50 mL)
3. washThe combined organic layers were washed with brine
4. dry with materialdried over Na2SO4
5. customevaporated