1-Bromo-3-methylbutane → HCID 78912157, compound

Temperature

65 °C

To a solution of 2,2-diethoxyethanamine 2.91 ml (20 mmol) in acetonitrile 50 ml, potassium carbonate 2.0 g (15 mmol) and a solution of isoamylbromide 1.26 ml (10 mmol) in acetonitrile 20 ml were added and the mixture was stirred at 65° C. overnight. The reaction mixture was concentrated in vacuo and the residue was diluted with ethyl acetate 100 ml and washed with water 100 ml and brine 100 ml. The organic phase was dried over magnesium sulfate and filtered. The filtrate was concentrated in vacuo and the residue was purified on Büch silica gel column chromatography (n-hexane:ethyl acetate=90:10 to 80:20) to obtain the title compound 1.57 g (77%).

1. concentrationThe reaction mixture was concentrated in vacuo
2. additionthe residue was diluted with ethyl acetate 100 ml
3. washwashed with water 100 ml and brine 100 ml
4. dry with materialThe organic phase was dried over magnesium sulfate
5. filtrationfiltered
6. concentrationThe filtrate was concentrated in vacuo
7. customthe residue was purified on Büch silica gel column chromatography (n-hexane:ethyl acetate=90:10 to 80:20)

ORD record

ord-f5c8dfb753f149a6a5ed96326552f546

Source dataset

uspto-grants-2015_05

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US09040531B2