反应详情

温度

-10 °C

DIPEA (4.1 mL) was added to a solution of 4,6-dichloropyrimidine-5-carbaldehyde (intermediate 8) (4.2 g) in DCM (85 mL) under an inert atmosphere. The solution was cooled to −10° C. and methylthioglycolate (2.1 mL) in DCM (40 mL) was added dropwise over 30 minutes. The reaction mixture was allowed to warm to ambient temperature over 2 hours, washed with water (4×50 mL), dried (MgSO4), filtered and concentrated in vacuo to give the title compound as an orange oil which later solidified (5.4 g, 92%);

1. temperatureto warm to ambient temperature over 2 hours
2. washwashed with water (4×50 mL)
3. dry with materialdried (MgSO4)
4. filtrationfiltered
5. concentrationconcentrated in vacuo