Ammonium Chloride → 4-Chloro-6-(methylsulfanyl)pyrimidine

Temperature

0 °C

To 10 ml of an ethanol solution of 1.5 g of 4,6-dichloropyrimidine was slowly added 0.78 g of sodium thiomethoxide at 0° C., followed by stirring at 0° C. for 7 hours. A saturated aqueous ammonium chloride solution was added to the reaction mixture and concentrated under reduced pressure. The residue was extracted three times with chloroform. The chloroform layers were combined, washed with water, dried over anhydrous magnesium sulfate, and then concentrated. The residue was subjected to silica gel column chromatography to give 1.1 g of 4-chloro-6-methylthiopyrimidine.

1. customat 0° C.
2. concentrationconcentrated under reduced pressure
3. extractionThe residue was extracted three times with chloroform
4. washwashed with water
5. dry with materialdried over anhydrous magnesium sulfate
6. concentrationconcentrated

ORD record

ord-e2b73363cfc64bf1a062b84456085e18

Source dataset

uspto-grants-2005_01

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US06838463B2