反应详情

{6-[4-(4-Benzyl-phthalazin-1-yl)-piperazin-1-yl]-pyridin-3-yl}-methanol (75 mg, 0.182 mmol) is dissolved in THF (1 mL) and added to a flask containing NaH (7.5 mg, 0.188 mmol). Stir 1 h at room temperature. Add dimethyl carbamoyl chloride (22 mg, 2.096 mmol) and stir for 16 h at room temperature. Incomplete conversion observed. Reaction is heated to 60° C. and stirred 16 h. Add additional NaH (7.5 mg, 0.188 mmol) is added and reaction quickly reaches 95% conversion. Concentrate reaction mixture in vacuo. The residue is purified by flash chromatography on silica gel (MeOH/CH2Cl2) to afford the title compound (24 mg, 27%).

1. additionadded to a flask
2. customReaction
3. temperatureis heated to 60° C.
4. stirringstirred 16 h
5. additionis added
6. customreaction quickly reaches 95% conversion
7. concentrationConcentrate
8. customreaction mixture in vacuo
9. customThe residue is purified by flash chromatography on silica gel (MeOH/CH2Cl2)