Hydrochloric Acid → 2,4-Dichloro-6-ethyl-5-fluoropyrimidine

To the solution obtained as the product of part (ii) was added a solution of potassium permanganate (23 g) in water (260 ml) over 2 hours, keeping the temperature of the reaction below 20° C. 5N hydrochloric acid (30 ml) was then added followed by a solution of sodium metabisulphite (14 g) in water (42 ml). After decolourisation of the mixture the product was extracted into ethyl acetate (250 ml). The organic layer was then concentrated to give an oil. The oil was partitioned between dichloromethane (50 ml) and 2N sodium hydroxide (105 ml) and the organic layer was washed with 5% brine (100 ml). The organic layer was concentrated to give a solution of the title compound which was used directly in the next step.

1. customthe temperature of the reaction below 20° C
2. extractionAfter decolourisation of the mixture the product was extracted into ethyl acetate (250 ml)
3. concentrationThe organic layer was then concentrated
4. customto give an oil
5. customThe oil was partitioned between dichloromethane (50 ml) and 2N sodium hydroxide (105 ml)
6. washthe organic layer was washed with 5% brine (100 ml)
7. concentrationThe organic layer was concentrated

ORDレコード

ord-0a913e889ca449e393953340fb0ba119

出典データセット

uspto-grants-1996_10

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US05567817