Aluminium lithium hydride → HCID 73236150, compound

Temperature

0 °C

31 g (120.0 mmol) of 3,3,3-trifluoro-2-[(2-hydroxy-1-phenylethyl)amino]-2-methylpropionitrile Example 242A were initially charged in tert-butyl methyl ether (3.1 l), the mixture was cooled to 0° C., 18.25 g (480.2 mmol) of lithium aluminium hydride were added and the reaction mixture was stirred at RT for 16 h. The mixture was then cooled to 0° C. and initially quenched with 24 ml of water, and 24 ml of 15% strength aqueous potassium hydroxide solution and 48 ml of water were then added. The mixture formed was filtered through silica gel and washed with tert-butyl methyl ether. The organic phase was separated off, dried over sodium sulphate, filtered and concentrated. This gave 29.2 g (83% of theory, purity 89%) of the target compound.

1. temperatureThe mixture was then cooled to 0° C.
2. custominitially quenched with 24 ml of water, and 24 ml of 15% strength aqueous potassium hydroxide solution and 48 ml of water
3. additionwere then added
4. customThe mixture formed
5. filtrationwas filtered through silica gel
6. washwashed with tert-butyl methyl ether
7. customThe organic phase was separated off
8. dry with materialdried over sodium sulphate
9. filtrationfiltered
10. concentrationconcentrated

ORD record

ord-3650eb8381214002a767757ae95a172c

Source dataset

uspto-grants-2015_09

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US09126998B2