反应详情

Prepared from 5-(4-Methyl-5-trifluoromethyl-isoxazol-3-yl)-thiophene-2-carboxylic acid and cyclopropylmethylamine by the method described in Example 2 Method B. The reaction mixture was evaporated in vacuo, triturated and filtered with the aid of water, then washed with an aqueous 1 N hydrochloric acid solution followed by water. The crude solid was then triturated with a 25% EtOAc/hexanes solution (3×1 mL) and air dried to afford product as a colorless solid (110 mg, 67%). 1H NMR (CDCl3) 0.27-0.32 (m, 2H), 0.55-0.61 (m, 2H), 1.03-1.12 (m, 1H), 2.37 (d, J=0.9, 3H), 3.31 (d, J=5.7, 1H), 3.33 (d, J=5.7, 1H), 6.23 (br s, 1H), 7.50 (d, J=4.0, 1H), 7.56 (d, J=4.0, 1H). 19F NMR −63.1. LC/MS 6.5 min, [M+1]+ 331.

1. customThe reaction mixture was evaporated in vacuo
2. customtriturated
3. filtrationfiltered with the aid of water
4. washwashed with an aqueous 1 N hydrochloric acid solution
5. customThe crude solid was then triturated with a 25% EtOAc/hexanes solution (3×1 mL) and air
6. customdried