反应详情

温度

3 °C

To a stirred solution of 10-chloro-4,4-diethyl-2-propan-2-yl-2,6,9,11-tetrazabicyclo[5.4.0]undeca-7,9,11-trien-5-one (Intermediate 197; 2.7 g, 9.1 mmol) in DMA (50 mL) under nitrogen was added methyl iodide (0.627 mL, 10.0 mmol). The mixture was cooled on an ice/water bath to 3° C., and sodium hydride (60% mineral oil dispersion; 0.567 g, 11.8 mmol) added in one portion. The reaction was stirred overnight. The reaction was evaporated to dryness to afford a yellow solid, this was quenched with saturated NH4Cl(aq) (50 mL), extracted with DCM (3×100 mL), dried (MgSO4) and evaporated to yield a yellow solid. This was dissolved in a minimum amount of DCM, diethyl ether was added and the system was sonicated to afford an off white solid. (2.24 g, 80%)

1. customThe reaction was evaporated to dryness
2. customto afford a yellow solid
3. customthis was quenched with saturated NH4Cl(aq) (50 mL)
4. extractionextracted with DCM (3×100 mL)
5. dry with materialdried (MgSO4)
6. customevaporated
7. customto yield a yellow solid
8. additionwas added
9. customthe system was sonicated
10. customto afford an off white solid