反应详情

To a solution of 396A (1.85 g, 4.50 mmol) in THF (25 ml) was added a solution of 3M MeMgBr in Et2O (15 ml, 45 mmol) slowly at 0° C. The reaction mixture was warmed to rt, then heated at 50° C. for 30 min. After cooled to 0° C., the reaction was quenched with aqueous NH4Cl, extracted with EtOAc, dried and concentrated to give 1.8 g of crude 396 as a yellow solid. It has a retention time 6.49 min. (Column: HTS, 5 u, 4.6×50 mm; Gradient: 5-100% B in 8.0 min; A=0.1% TFA/H2O; B=0.1% TFA/CH3CN; Run time 10 min; Det: 215 nM; FR: 1.2 ml/min); MS Found: (M−H)+=397.4

1. temperatureheated at 50° C. for 30 min
2. temperatureAfter cooled to 0° C.
3. customthe reaction was quenched with aqueous NH4Cl
4. extractionextracted with EtOAc
5. customdried
6. concentrationconcentrated