tert-butyl 3,5-bis(trifluoromethyl)phenylcarbamate synthesis
- Product Name:tert-butyl 3,5-bis(trifluoromethyl)phenylcarbamate
- CAS Number:26684-29-7
- Molecular formula:C13H13F6NO2
- Molecular Weight:329.24
Yield:26684-29-7 75.4%
Reaction Conditions:
with dmap;triethylamine in toluene at 100; for 48 h;
Steps:
1 (3,5-Bis-trifluoromethyl-phenyl)-carbamic acid tert-butyl ester (2):
(3,5-Bis-trifluoromethyl-phenyl)-carbamic acid tert-butyl ester (2): [00213] To a solution of (3,5-Bis-trifluoromethyl)aniline (1 , 10.0 g, 43.64 mmol) in toluene (100mL) was added triethylamaine (7.3 mL), DMAP (0.54 g) and Boc)2O (1 1 .5 g, 52.72 mmol). The mixture was stirred at 100°C for 48 hrs. After cooling to room temperature, the reaction mixture was diluted with H2O (200 mL). The aqueous phase was extracted twice with 150 ml. The organic layer was washed with Na2C03 (sat.) solution and brine. Organic layer was concentrated and the crude material was purified by silica gel chromatography (6-10% EtOAc/hexanes) to give (3,5-Bis-trifluoromethyl-phenyl)-carbamic acid tert-butyl ester (2) as a white solid (8 g, 75.4%). 1 H-NMR (300 MHz, CDCI3): 6 7.86 (s, 2H), 7.57 (s, 1 H), 6.79 (s, 1 H), 1 .53 (s, 9H).
References:
WO2017/70795,2017,A1 Location in patent:Paragraph 00213
328-74-5
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