反应详情

A suspension of pyrido[3,4-d]pyrimidin-4-ol (33)(1.47 g, 10 mmol) in thionylchloride (30 ml) and dimethylformamide (50 μl, cat.) was heated to reflx (90° C.) for 1 hour. The mixture was then cooled and concentrated in vacuo and then diluted with CH2Cl2 (50 ml) which caused a suspension to form. The solid was removed by filtration, washed with cold CH2Cl2 (10 ml) to give the title compound (1.65 g, 99.4%) in sufficiently pure form to be used without any further purification. m/z (LC-MS, ESP): 166 [M+H]+, R/T=2.82 mins.

1. temperaturewas heated
2. custom(90° C.)
3. customfor 1 hour
4. temperatureThe mixture was then cooled
5. concentrationconcentrated in vacuo
6. additiondiluted with CH2Cl2 (50 ml) which
7. customto form
8. customThe solid was removed by filtration
9. washwashed with cold CH2Cl2 (10 ml)