1,2-Dichloroethane → HCID 88929351, compound

A mixture of 4-(trifluoromethoxy)butanoic acid (1.0 g, 5.81 mmol) and HOBt (1.157 g, 7.55 mmol) in MeCN (20 mL) was treated with EDC (1.448 g, 7.55 mmol) and stirred at RT for 2 h. Ammonium hydroxide (˜15M, 0.7 mL, ˜10.5 mmol) was added and the mixture stirred at RT for 20 h. The mixture was treated with Et2O, water and brine, the layers separated and the organic layer dried over Na2SO4 and concentrated to afford 4-(trifluoromethoxy)butanamide (1.024 g, 103%) as a white solid. 1H NMR (400 MHz, DMSO-d6): δ 7.30 (s, 1H), 6.78 (s, 1H), 4.04 (t, J=6.4 Hz, 2H), 2.13 (t, J=7.4 Hz, 2H), 1.82 (m, 2H).

1. stirringthe mixture stirred at RT for 20 h
2. customthe layers separated
3. dry with materialthe organic layer dried over Na2SO4
4. concentrationconcentrated

ORD record

ord-68f874f477ff43eebb3b60cc2bb42485

Source dataset

uspto-grants-2016_07

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US09382228B2