Ethyl Acetate → HCID 59596400, compound

Participants

Reaction Conditions

Reaction Steps

A mixture of 300 mg (0.65 mMol) of 7-hydroxy-2,3,4,5-tetrahydro-benzo[b]azepine-1-carboxylic acid [3-trifluoromethyl-4-(4-methylpiperazin-1-ylmethyl)-phenyl]-amide (Step 12.2), 106 mg (0.65 mMol) 2-amino-4,6-dichloro-pyrimidine and 26 mg (0.65 mMol) NaOH in 2 ml acetone, 2 ml H2O and 1.2 ml DMEU is stirred at 60° C. for 12 h. Then the suspension is dissolved by addition of water and EtOAc, the aqueous phase separated off and extracted twice with EtOAc. The organic layers are washed with water and brine, dried (Na2SO4) and concentrated. Reversed phase MPLC (Gilson system) gives the title compound: MS: [M+1]+=590/592; HPLC: AtRet=12.7.

Provenance & Evidence