反应详情

A solution containing (±)-1-(3-amino-4-cyano-benzyl)-4-(6-chloro-benzo[b]thiophene-2-sulfonyl)-6-oxo-piperazine-2-carboxylic acid methyl ester (42 mg, 0.08 mmol), EXAMPLE 99, 1,3,5-triazine (40 mg, 0.48 mmol), and glacial HOAc (30 mg, 0.48 mmol) in absolute EtOH (1 mL) is maintained at reflux for 16 hours. The reaction mixture is concentrated and then dissolved in water/CH3CN and purified by reverse-phase HPLC [Buffer A: water w/0.1% TFA; Buffer B: CH3CN w/0.1% TFA; Gradient: 0% B to 60% B over 30 min] to provide 17 mg (32%) of the title compound as a white solid.

1. temperatureis maintained
2. temperatureat reflux for 16 hours
3. concentrationThe reaction mixture is concentrated
4. dissolutiondissolved in water/CH3CN
5. custompurified by reverse-phase HPLC [Buffer A: water