2,4,5-Trichloropyrimidine → 2,5-Dichloro-4-methoxypyrimidine

Sodium methoxide (295 mg, 5.45 mmol) was taken up in methanol (13.6 ml) and 2,4,5-trichloropyrimidine (500 mg, 2.73 mmol) was added. The mixture was stirred at room temperature overnight. The resulting mixture was concentrated under reduced pressure. The resulting residue was diluted with diethyl ether, washed with 1:1 water:saturated aqueous ammonium chloride. The organic layer was dried over magnesium sulfate, filtered, and concentrated under reduced pressure. Purification by Combiflash (0-10% diethyl ether/hexanes) afforded 280 mg (1.56 mmol, 57%) of 2,5-dichloro-4-methoxypyrimidine as a white solid.

1. concentrationThe resulting mixture was concentrated under reduced pressure
2. additionThe resulting residue was diluted with diethyl ether
3. washwashed with 1:1 water
4. dry with materialThe organic layer was dried over magnesium sulfate
5. filtrationfiltered
6. concentrationconcentrated under reduced pressure
7. customPurification by Combiflash (0-10% diethyl ether/hexanes)

ORDレコード

ord-e5b541d08cd24fa29b3bf6d785751341

出典データセット

uspto-grants-2014_05

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US08735417B2