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With methanesulfonyl chloride; 1,8-diazabicyclo[5.4.0]undec-7-ene In toluene at 110℃; for 2 h;
Example 18C 1-tert-butyl 4-ethyl 2,3,6,7-tetrahydro-1H-azepine-1,4-dicarboxylate To a solution of EXAMPLE 18B (21 g, 73 mmol), DBU (22 g, 146 mmol) in toluene (200 mL) was added dropwise MsCl (14.56 g, 128 mmol). After the dropwise addition was completed, the mixture was stirred at 110° C. for 2 h, and cooled to room temperature, and then water (200 mL) was added to quench. The aqueous layer was extracted with EtOAc (200 mL*2). The combined organic layers were washed with water, brine, dried over Na2SO4, filtered and evaporated. The residue was purified by column chromatograph on silica gel to provide the title compound (13 g, yield: 66percent). LCMS (ESI) m/z: 270 (M+1).
With methanesulfonyl chloride; 1,8-diazabicyclo[5.4.0]undec-7-ene; In toluene; at 110℃; for 2h;
Example 18C 1-tert-butyl 4-ethyl 2,3,6,7-tetrahydro-1H-azepine-1,4-dicarboxylate To a solution of EXAMPLE 18B (21 g, 73 mmol), DBU (22 g, 146 mmol) in toluene (200 mL) was added dropwise MsCl (14.56 g, 128 mmol). After the dropwise addition was completed, the mixture was stirred at 110 C. for 2 h, and cooled to room temperature, and then water (200 mL) was added to quench. The aqueous layer was extracted with EtOAc (200 mL*2). The combined organic layers were washed with water, brine, dried over Na2SO4, filtered and evaporated. The residue was purified by column chromatograph on silica gel to provide the title compound (13 g, yield: 66%). LCMS (ESI) m/z: 270 (M+1).
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