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

Temperature

150 °C

3.33 g (30.0 mmol) 2-fluoro-4-methylpyridine are initially introduced into 40 ml 2-ethoxyethanol, 14.6 ml (15.0 g, 300 mmol) hydrazine hydrate are added to the solution and the mixture is stirred at the boiling point (150° C. bath temperature) for 16 h. Thereafter, the reaction solution is concentrated on a rotary evaporator, the residue is added to 100 ml water and the mixture is extracted with ethyl acetate (three times with 100 ml each time). The combined organic phases are dried over sodium sulfate, filtered and concentrated. The residue obtained is dried in vacuo.

1. additionare added to the solution
2. concentrationThereafter, the reaction solution is concentrated on a rotary evaporator
3. additionthe residue is added to 100 ml water
4. extractionthe mixture is extracted with ethyl acetate (three times with 100 ml each time)
5. dry with materialThe combined organic phases are dried over sodium sulfate
6. filtrationfiltered
7. concentrationconcentrated
8. customThe residue obtained
9. customis dried in vacuo

ORD record

ord-5527f8720a414eabb11f020bdb79a122

Source dataset

uspto-grants-2015_03

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US08987261B2