Dichloromethane → 4-(1-Bromoethyl)-6-chloro-5-fluoropyrimidine

Temperatur

25 °C

A stirred mixture of the compound of part (v) (38.5 kg), azoisobutyronitrile (AIBN) (1.92 kg), N-bromosuccinimide (49 kg) and dichloromethane (198 L) was heated under reflux under nitrogen for 12 hours. The mixture was cooled to 25° C. and water (239 L) added. The layers were separated and the aqueous layer extracted with dichloromethane (120 L). The combined organic layers were washed with a solution of sodium metabisulphite (22.8 kg) in water (239 L), followed by water (239 L). The organic layer was concentrated under reduced pressure, toluene (240 L) was added and the resulting solution concentrated under reduced pressure to give the product as an oil (61.7 kg).

1. temperaturewas heated
2. temperatureunder reflux under nitrogen for 12 hours
3. customThe layers were separated
4. extractionthe aqueous layer extracted with dichloromethane (120 L)
5. washThe combined organic layers were washed with a solution of sodium metabisulphite (22.8 kg) in water (239 L)
6. concentrationThe organic layer was concentrated under reduced pressure, toluene (240 L)
7. additionwas added
8. concentrationthe resulting solution concentrated under reduced pressure

ORD-Eintrag

ord-0f9cb527900142f1be56796bd74836c9

Quelldatensatz

uspto-grants-2007_03

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US07193083B2