Ethyl Acetate → HCID 57382977, compound

Participants

Reaction Conditions

Reaction Steps

4-chloro-5-methyl-7H-pyrrolo[2,3-d]pyrimidine D4 (218 mg), N-{3-[(methyloxy)methyl]-4-piperidinyl}benzamide D35 (500 mg) and N,N-diisopropylethylamine (504 mg, 3.9 mmol) were dissolved in NMP (10 ml). The tube was sealed and the reaction carried out in the microwave. The reaction was heated at 150° C. for 3 hours. The reaction mixture was poured into ethyl acetate (120 ml), washed with water (3×30 ml), brine (2×30 ml). Organic layer collected and dried with MgSO4, filtered and solvent removed. Purification of the crude product by chromatography on silica gel eluting with DCM/MeOH 30/1 to give product. Repurified by prep-HPLC (column: x-bridge C18sun, 30×, 50 mm; mobile phase: A 10 mmol/L NH3.H2O B ACN; gradient: 35-40% ACN in 6-7 min. Rt 6.3 min to give the product E42 as a yellow solid in 86 mg. LCMS [M+H] [email protected] min (mixture of 2 isomers) (5 min run)

Provenance & Evidence