Reaktion #659465

Reaktionsgleichung

5-(4-Methyl-5-trifluoromethyl-isoxazol-3-yl)-thiophene-2-carboxylic acid

thiomopholine 1,1-dioxide

→

product

Ausbeute 80.0%

(1,1-Dioxo-1 lambda-6-thiomorpholin-4-yl)-[5-(4-methyl-5-trifluoromethyl-isoxazol-3-yl)-thiophen-2-yl]-methanone

Ausbeute 80.0%

Reaktionsbedingungen

Aufarbeitung

1. 1
   SonstigeThe reaction mixture was evaporated to a solid
2. 2
   Sonstigetriturated
3. 3
   Filtrationfiltered with the aid of water
4. 4
   Waschenwashed with a 1 N aqueous hydrochloric acid solution
5. 5
   Sonstigedried

Vorschrift

Prepared from 5-(4-Methyl-5-trifluoromethyl-isoxazol-3-yl)-thiophene-2-carboxylic acid and thiomopholine 1,1-dioxide by the method described in Example 2 Method B. 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 (157 mg, 80%). 1H NMR (DMSO-d6) 2.34 (d, J=1.7, 3H), 3.27 (obs m, 4H), 4.00 (m, 4H), 7.58 (d, J=3.5, 1H), 7.68 (d, J=4.0, 1H). 13C NMR (incomplete, F-coupled carbons obscured by baseline noise due to poor solubility) 8.0, ˜44 (br), 51.5, 116.6, 128.0, 130.0, 130.8, 139.6, 158.5, 162.7. 19F NMR −62.2. LC/MS 5.80 min, [M+1]+ 395.

Quelle