Methanol → HCID 68683076, compound

Participants

Reaction Steps

10-chloro-6-methyl-2-(2-morpholin-4-ylethyl)-2,6,9,11-tetrazabicyclo[5.4.0]undeca-7,9,11-trien-5-one (Intermediate 160; 95 mg, 0.29 mmol), -amino-3-methoxy-N-(1-methyl-4-piperidyl)benzamide (WO06/018220; 86 mg, 0.35 mmol) and p-toluenesulphonic acid monohydrate (110 mg, 0.58 mmol) were heated together in IPA (4 mL) by microwave irradiation at 150° C. for 20 minutes. The reaction mixture was loaded onto an SCX-2 (5 g) column pre-wet with methanol; the column was washed with methanol and the product eluted with 2M NH3/MeOH. Product containing fractions were combined and evaporated. The resultant material was purified by base modified reverse phase preparative HPLC to yield the title compound as a white solid (56 mg, 36%).

Provenance & Evidence