Water → 2,4-Dichloro-6-methoxypyrimidine

Temperature

0 °C

3.24 g of sodium methoxide dissolved beforehand in 13 ml of methanol are added dropwise to a solution of 11 g of 2,4,6-trichloropyrimidine in 140 ml of methanol cooled to 0° C. in an ice bath. The ice bath is withdrawn. The reaction medium is stirred at 0° C. for 45 minutes, and then the cooling bath is removed so as to allow the temperature to rise to ambient temperature. The reaction medium is concentrated under reduced pressure. The residue obtained is taken up with 30 ml of water and 100 ml of ethyl acetate. After settling out, the organic phase is dried over magnesium sulfate, filtered, and concentrated under reduced pressure so as to give an oil which is left to crystallize for 24 hours at ambient temperature. The product crystallizes in the form of needles in the middle of an oil. The needles are separated so as to give 3.94 g of 2,4-dichloro-6-methoxypyrimidine, the characteristics of which are the following:

1. customThe ice bath is withdrawn
2. customthe cooling bath is removed so as
3. customto rise to ambient temperature
4. concentrationThe reaction medium is concentrated under reduced pressure
5. customThe residue obtained
6. dry with materialthe organic phase is dried over magnesium sulfate
7. filtrationfiltered
8. concentrationconcentrated under reduced pressure so as
9. customto give an oil which
10. waitis left
11. customto crystallize for 24 hours at ambient temperature
12. customThe product crystallizes in the form of needles in the middle of an oil
13. customThe needles are separated so as

ORD record

ord-d4b91e00685b4133974790a0378d367c

Source dataset

uspto-grants-2015_09

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US09133168B2