Hydrazine hydrate (1:1) → (1,1-Dimethoxypropan-2-yl)hydrazine

Temperature

140 °C

6.25 g (34.1 mmol) of 2-bromo-1,1-dimethoxypropane and 6.65 ml (137 mmol) of hydrazine hydrate were stirred under reflux in an oil bath at 140° C. for 6 h. After cooling, the two-phase reaction mixture was extracted with 50 ml of tert-butyl methyl ether. The organic phase was filtered, the filtrate was concentrated on a rotary evaporator and the residue was dried under high vacuum. This gave 1.89 g (21% of theory) of a pale yellow oil which was reacted directly, without further purification, in the subsequent reaction.

1. temperatureAfter cooling
2. customthe two-phase reaction mixture
3. extractionwas extracted with 50 ml of tert-butyl methyl ether
4. filtrationThe organic phase was filtered
5. concentrationthe filtrate was concentrated on a rotary evaporator
6. customthe residue was dried under high vacuum
7. customThis gave 1.89 g (21% of theory) of a pale yellow oil which was reacted directly, without further purification, in the subsequent reaction

ORD record

ord-bfda85a739c94ee7a81ea9a7f302f9fe

Source dataset

uspto-grants-2016_07

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US09394309B2