反应详情

Use a method similar to the Example 347, using the 4:1 mixture of 3-tert-butoxycarbonyl-7-chloro-6-dimethylcarbamoylthio-2,3,4,5-tetrahydro-1H-benzo[d]azepine and 3-tert-butoxycarbonyl-7,9-dichloro-6-dimethylcarbamoylthio-2,3,4,5-tetrahydro-benzo[d]azepine with methyl 2-(bromomethyl)benzoate. Use a method similar to the General Procedure 1-4 and purify by preparative reverse phase HPLC (Column: Xterra Prep RP18 19×250 mm; solvent A: 10 mM aqueous ammonium carbonate, solvent B: acetonitrile; 30-100% B over 20 minutes; flow rate 25 mL/min). Use a method similar to the General Procedure 2-2, to give the title compound as a white solid. MS (ES+) m/z: 362 (M+H)+.

1. custompurify by preparative reverse phase HPLC (Column: Xterra Prep RP18 19×250 mm; solvent A: 10 mM aqueous ammonium carbonate, solvent B: acetonitrile; 30-100% B over 20 minutes; flow rate 25 mL/min)