2,2-二氯-1-(羟基甲基)环丙烷

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: In a sulfonation flask, 2.8 g (0.02 mol) of 2,2-dichlorocyclopropanmethanol are added to 40 ml of absolute tetrahydrofurane and under stirring 0.6 g (0.015 mol) NaH-dispersion is carefully added. After stirring for 1 hour at room temperature, a solution of 2.4 g (0.01 mol) 2-methylsulfanyl-3-propyl-3H-thieno[2.3-d]pyrimidin-4-one in 20 ml tetrahydrofurane was added within 2 minutes. After stirring for 4 hours at room temperature the solvent is removed in a water-jet vacuum and the residue is taken up in TBME and the mixture washed repeatedly with water. The TBME-phase is concentrated in the water-jet vacuum and subsequently the excess 2,2-dichlorocyclopropylmethanol destined in high vacuum. 3.0 g of 2-(2,2-dichloro-cyclopropylmethoxy)-3-propyl-3H-thieno[2.3-d]pyrimidin-4-one are obtained in the form of a white powder having a melting point of 64-66° C. is carefully added After stirring for 4 hours at room temperature the solvent is removed in a water-jet vacuum the mixture washed repeatedly with water The TBME-phase is concentrated in the water-jet vacuum