反应详情

温度

180 °C

To a solution of 4-phenylpiperidine-4-carboxylic acid from step A (0.74 g, 3.1 mmol) in isopropanol (10 mL), was added 4-chloro-5-methyl-7H-pyrrolo[2,3-d]pyrimidine (0.52 g, 3.1 mmol) and triethylamine (1.0 mL, 9.8 mmol). The reaction mixture was heated at 180° C. for 180 minutes under microwave condition, and then concentrated under vacuum. The residue was dissolved in ice water and neutralized to pH 4 by addition of 1 N aq. HCl. The product was isolated by filtration and dried under vacuum for 3 hours at 65° C. to give the title compound (62%) as a brown solid. MS (ES+) [M+H]+=336.

1. concentrationconcentrated under vacuum
2. dissolutionThe residue was dissolved in ice water and neutralized to pH 4 by addition of 1 N aq. HCl
3. customThe product was isolated by filtration
4. customdried under vacuum for 3 hours at 65° C.