反应详情

Prepared from 5-(5-Trifluoromethyl-4-methyl-isoxazol-3-yl)-thiophene-2-carboxylic acid and morpholine by the method described in Example 2 Method B reversing the order of addition such that solid acid chloride was added to a THF solution of triethylamine and piperidine derivative. The reaction mixture was evaporated to a solid, triturated and filtered with the aid of water, then washed with a 1 N aqueous hydrochloric acid solution followed by water. The solid was air dried to afford product as a colorless solid (66 mg, 95%). 1H NMR (CDCl3) 2.34 (d, J=1.3, 3 H), 3.71-3.77 (m, 8 H), 7.32 (d, J=4.0, 1 H), 7.43 (d, J=4.0, 1 H). 13C NMR 7.9, ˜48 (br), 67.0, 114.7, 118.7 (q, J=271), 128.0, 129.5, 131.7, 139.5, 157.9, 162.8. 19F NMR −63.2. LC/MS 5.93 min, [M+1]+ 347.

1. customThe reaction mixture was evaporated to a solid
2. customtriturated
3. filtrationfiltered with the aid of water
4. washwashed with a 1 N aqueous hydrochloric acid solution
5. customdried