Diisopropylethylamine → Tert-butyl 4-{[6-chloro-2-(trifluoromethyl)pyrimidin-4-yl]amino}piperidine-1-carboxylate

tert-Butyl 4-aminopiperidine-1-carboxylate (1.4 g, 7.1 mmol, Aldrich) was dissolved in methylene chloride (10. mL) and to this solution was added N,N-diisopropylethylamine (2.5 mL, 14 mmol) and 4,6-dichloro-2-(trifluoromethyl)pyrimidine (1.7 g, 7.8 mmol, Synchem). The reaction was stirred overnight. The mixture was diluted with water and the product was extracted with EtOAc. The organic layer was washed twice with water, once with brine, dried over sodium sulfate, filtered and concentrated to afford product which was used without further purification in Step 2. LCMS (M+H)+: 381.1.

1. extractionthe product was extracted with EtOAc
2. washThe organic layer was washed twice with water, once with brine
3. dry with materialdried over sodium sulfate
4. filtrationfiltered
5. concentrationconcentrated
6. customto afford product which
7. customwas used without further purification in Step 2

ORD record

ord-52d7c2cab18c4fe4b12dea61ef15a833

Source dataset

uspto-grants-2015_11

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US09193733B2