反应详情

As an alternative to the previous synthesis, the title compound was prepared starting from a solution of 4-(3,5-dichloro-pyridin-4-ylmethyl)-7-methoxy-1,2-dihydro-phthalazine (2 g, 6.2 mmoles), prepared as described in example 22, in dry THF (60 ml) under stirring and dry N2 at 0° C. The mixture was added with triethylamine (1.57 g, 15.5 mmoles), then with acetyl chloride (0.44 ml, 6.2 mmoles). After 10 minutes the mixture was brought to room temperature and kept at such temperature for 2.5 hours, then poured into water/ice and extracted more times with CH2Cl2. The organic phases were washed with 5% NaOH and water, anhydrified and brought to dryness to give a solid which, by crystallisation from acetonitrile (70 ml), gave 1.95 g of the title compound having the same physochemical characteristics set forth at point A.

1. customAs an alternative to the previous synthesis
2. customthe title compound was prepared
3. customprepared
4. customat 0° C
5. waitkept at such temperature for 2.5 hours
6. extractionextracted more times with CH2Cl2
7. washThe organic phases were washed with 5% NaOH and water
8. customto give a solid which
9. customby crystallisation from acetonitrile (70 ml)