反应详情

A solution of compound 20 (900 mg, 1.800 mmol), 3,3-dimethylbutyraldehyde (904 μl, 7.20 mmol), formic acid (552 μl, 14.40 mmol) and TEA (251 μl, 1.800 mmol) in acetonitrile (45 ml) is irradiated with microwaves (140° C., 15 minutes). The reaction is partitioned between AcOEt and NaHCO3 solution. The organic layers are then washed with brine, dried over Na2SO4 and filtered. The solvent is evaporated to give a oil which is purified by silica gel chromatography (from DCM:MeOH 100:0 to 98.5:1.5) to give the title compound (721 mg, 1.316 mmol, 73.1% yield).

1. customThe reaction is partitioned between AcOEt and NaHCO3 solution
2. washThe organic layers are then washed with brine
3. dry with materialdried over Na2SO4
4. filtrationfiltered
5. customThe solvent is evaporated
6. customto give a oil which
7. customis purified by silica gel chromatography (from DCM:MeOH 100:0 to 98.5:1.5)