反应详情

To a mixture of (4-methylamino-phenyl)-(1,3,3-trimethyl-6-aza-bicyclo[3.2.1]oct-6-yl)-methanone (0.7 g, 2.44 mmol), DCM (40 ml) and TEA (0.7 ml, 4.89 mmol) was added methansulfonyl chloride (285 μl, 3.67 mmol). The resulting mixture was stirred for 4 hrs. at room temperature followed by evaporation of the volatiles in vacuo. The residue was dissolved in diethyl ether (10 ml), washed with water (2×10 ml) evaporated and the residue purified by column chromatography (silica gel) using a mixture of EtOAc-Heptane (1:1) as eluent. Pure fractions were collected and evaporated to dryness. The residue was crystallized from diethyl ether (10 ml), filtered off and dried in vacuo at 50° C. affording 0.45 g (51%) of the title compound as a solid.

1. customat room temperature followed by evaporation of the volatiles in vacuo
2. dissolutionThe residue was dissolved in diethyl ether (10 ml)
3. washwashed with water (2×10 ml)
4. customevaporated
5. customthe residue purified by column chromatography (silica gel)
6. additiona mixture of EtOAc-Heptane (1:1) as eluent
7. customPure fractions were collected
8. customevaporated to dryness
9. customThe residue was crystallized from diethyl ether (10 ml)
10. filtrationfiltered off
11. customdried in vacuo at 50° C.