1-氯-3,3,3-三氟丙酮

反应条件: temp:120.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: 5 g (28.5 mmol) of 6-chloro-2-(methylthio)pyrimidine-4-amine and 6.26 g (42.7 mmol) of 3-chloro-1,1,1-trifluoropropanone are dissolved in 200 ml of DMF and heated at 120° C. for 16 h. After the reaction is complete, water is added and the mixture is extracted three times with ethyl acetate. The combined organic phases are dried over sodium sulphate and the product is purified by silica gel chromatography. Drying under high vacuum results in 3.5 g (45% of theory) of the product as a solid. the mixture is extracted three times with ethyl acetate The combined organic phases are dried over sodium sulphate the product is purified by silica gel chromatography Drying under high vacuum

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: A mixture of 4, 5, 6-trichloropyridine-2-carbothioamide (2.85 g, 11.8 mmol) and 1-chloro-3,3,3-trifluoroacetone (2.59 g, 17.7 mmol) in glacial acetic acid (25 mL) was heated at reflux for 4 hours. Upon cooling, the solids formed were filtered and washed with water (3×100 mL) and sodium bicarbonate (3×50 mL). The solids were then dissolved in dichloromethane and the organic phase was washed with brine (150 mL), and dried (MgSO4). The solvent was removed and the residue purified by preparative liquid chromatography (90% acetonitrile in water) to give 2,3,4-trichloro-6-[5-(trifluoromethyl)-1,3-thiazol-2-yl]pyridine (0.70 g, 2.1 mmol); 1H NMR (CDCl3) δ 7.91 (s, 1H); 8.29 (s, 1H) and give 2,3,4-trichloro-6-[4-(trifluoromethyl)-1,3-thiazol-2-yl]pyridine (0.20 g, 0.6 mmol); 1H NMR (CDCl3) δ 8.24 (1H, s), 8.39 (1H, s). was heated at reflux for 4 hours Upon cooling the solids formed were filtered washed with water (3×100 mL) and sodium bicarbonate (3×50 mL) The solids were then dissolved in dichloromethane the organic phase was washed with brine (150 mL) dried (MgSO4) The solvent was removed the residue purified by preparative liquid chromatography (90% acetonitrile in water)

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: Prepared according to the procedure described in Example 6, Step 1, using the following starting materials: 3-bromothiophenol and 3-chloro-1,1,1-trifluoropropane-2-one. Prepared