Hydrazine hydrate (1:1) → 2-Hydrazinyl-4-methylpyridine

3.3 g (30.0 mmol) of 2-fluoro-4-methylpyridine are initially charged in 40 ml of ethylene glycol monoethyl ether, 14.6 ml (15.0 g, 300 mmol) of hydrazine hydrate are added to the solution and the mixture is stirred at boiling point (bath temperature 150° C.) for 16 h. The reaction solution is then concentrated on a rotary evaporator, and the residue is added to 100 ml of water and extracted with ethyl acetate (three times 100 ml each). The combined organic phases are dried over sodium sulfate, filtered and concentrated. The residue obtained is dried under reduced pressure.

1. custompoint (bath temperature 150° C.)
2. customfor 16 h
3. concentrationThe reaction solution is then concentrated on a rotary evaporator
4. additionthe residue is added to 100 ml of water
5. extractionextracted with ethyl acetate (three times 100 ml each)
6. dry with materialThe combined organic phases are dried over sodium sulfate
7. filtrationfiltered
8. concentrationconcentrated
9. customThe residue obtained
10. customis dried under reduced pressure

ORD record

ord-53caf575ccc747f1a4bef58efc644f4b

Source dataset

uspto-grants-2013_12

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US08609698B2