反应详情

A suspension under N2 of trifluoro-methanesulfonic acid 1-(3,5-dichloro-pyridin-4-ylmethyl)-6-methoxy-phthalazin-5-yl ester (5 g, 10.68 mmoles), prepared as described in example 73, benzyl-methyl-prop-2-ynyl-amine (2.16 ml, 12.82 mmoles) and diethylamine (100 ml) was added under stirring with bis(triphenylphosphine)PdCl2 (150.2 mg, 0.214 mmole) and CuI (40.75 mg, 0.214 mmole). The mixture was refluxed for 6 hours, brought to dryness and the residue flash chromatographed (eluent: ethyl acetate) to give a solid which was dissolved in CH2Cl2/CH3OH 1:1 (50 ml), acidified with a solution of HCl in ethyl acetate and brought to dryness. The residue was dissolved in CH2Cl2 (100 ml), brought to dryness again, triturated in ethyl acetate (150 ml), filtered and dried in oven under vacuum at 40° C. to give 5.22 g of the title compound (yield: 83%).

1. additionwas added
2. temperatureThe mixture was refluxed for 6 hours
3. customthe residue flash chromatographed (eluent: ethyl acetate)
4. customto give a solid which
5. customtriturated in ethyl acetate (150 ml)
6. filtrationfiltered
7. customdried in oven under vacuum at 40° C.