Trifluoroacetic anhydride → 1-(4-Bromo-5-methyl-thiophen-2-yl)-3-(3,5-dichloro-phenyl)-4,4,4-trifluoro-but-2-en-1-one
반응식
FC(F)(F)C(OC(=O)C(F)(F)F)=O.[Br:14][C:15]1[CH:16]=[C:17]([C:21](=[O:37])[CH2:22][C:23]([C:29]2[CH:34]=[C:33]([Cl:35])[CH:32]=[C:31]([Cl:36])[CH:30]=2)(O)[C:24]([F:27])([F:26])[F:25])[S:18][C:19]=1[CH3:20]>C(N(CC)CC)C>[Br:14][C:15]1[CH:16]=[C:17]([C:21](=[O:37])[CH:22]=[C:23]([C:29]2[CH:34]=[C:33]([Cl:35])[CH:32]=[C:31]([Cl:36])[CH:30]=2)[C:24]([F:27])([F:25])[F:26])[S:18][C:19]=1[CH3:20]참가 물질
4
실험 절차
Triethylamine (53 ml) and trifluoracetic anhydride (38 ml) are added to a solution of -(4-bromo-5-methyl-thiophen-2-yl)-3-(3,5-dichloro-phenyl)-4,4,4-trifluoro-3-hydroxy-butan-1-one (110 g, 77% purity) at 0° C. After 12 hours at room temperature, the reaction is quenched with water (200 ml) and a saturated aqueous solution of NaHCO3. The aqueous phase is separated and further extracted with two times dichloromethane. The organic phases are combined, washed with water, dried over MgSO4 and concentrated in vacuo to yield 1-(4-bromo-5-methyl-thiophen-2-yl)-3-(3,5-dichloro-phenyl)-4,4,4-trifluoro-but-2-en-1-one (95 g, 71% purity) as a brown oil. The crude product is used without further purification.