Methyl 4,4,4-trifluoro-2-hydroxybutanoate → 4,4,4-Trifluoro-2-hydroxybutanamide

A solution of 12-3 (200 mg, 1.16 mmol) in 7N NH3/MeOH (10 mL) was heated at 70° C. overnight. The reaction mixture was filtered, and the filtrate was concentrated to dryness. The residue was dissolved in 1,2-dimethoxyethane (10 mL) and filtered to remove insolubles. The filtrate was concentrated to dryness to afford Intermediate 12. 1H NMR (500 MHz, DMSO-d6) δ 7.40 (br s, 1H), 7.34 (br s, 1H), 5.93 (m, 1H), 4.10 (m, 1H), 2.64-2.65 (m, 1H), 2.40-2.41 (m, 1H).

1. filtrationThe reaction mixture was filtered
2. concentrationthe filtrate was concentrated to dryness
3. dissolutionThe residue was dissolved in 1,2-dimethoxyethane (10 mL)
4. filtrationfiltered
5. customto remove insolubles
6. concentrationThe filtrate was concentrated to dryness

ORD record

ord-20dbfbff0a8c4a75b6880e7ff4c3a084

Source dataset

uspto-grants-2016_08

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US09428492B2