3,3,3-trifluoro-2-methyl-2-(trifluoromethyl)propan-1-ol

反応条件: temp:0.00; pressure:0.00; stir:

反応条件: temp:0.00; pressure:0.00; stir:

反応条件: temp:0.00; pressure:0.00; stir:

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: To 2,2-bis(trifluoromethyl)propanol (4.34 g, 22.1 mmol) in DCM (100 mL) at 0° C. add with stirring triethylamine (6.2 mL, 44 mmol) followed by methanesulfonyl chloride (2.6 mL, 33 mmol). After 15 min at 0° C. dilute with water and extract three times with EtOAc. Dry over anhydrous Na2SO4 and concentrate in vacuo to give the crude desired intermediate as a yellow oil (6.16 g, 100%). extract three times with EtOAc Dry over anhydrous Na2SO4 concentrate in vacuo

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: To 2,2-bis(trifluoromethyl)propanol (4.34 g, 22.1 mmol) in DCM (100 mL) at 0° C. add with stirring triethylamine (6.2 mL, 44 mmol) followed by methanesulfonyl chloride (2.6 mL, 33 mmol). After 15 min at 0° C. dilute with water and extract three times with EtOAc. Dry over anhydrous Na2SO4 and concentrate in vacuo to give the crude desired intermediate as a yellow oil (6.16 g, 100%). extract three times with EtOAc Dry over anhydrous Na2SO4 concentrate in vacuo

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: To 2,2-bis(trifloromethyl)propanol (4.34 g, 22.1 mmol) in DCM (100 mL) at 0° C. add with stirring triethylamine (6.2 mL, 44 mmol) followed by methanesulfonyl chloride (2.6 mL, 33 mmol). After 15 min at 0° C. dilute with water and extract three times with EtOAc. Dry over anhydrous Na2SO4 and concentrate in vacuo to give the crude desired intermediate as a yellow oil (6.16 g, 100%). extract three times with EtOAc Dry over anhydrous Na2SO4 concentrate in vacuo

反応条件: temp:100.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: 3,3,3-Trifluoro-2-methyl-2-trifluoromethyl-propan-1-ol, 1 gm, 5.1 mM, and Dess-Martin Periodinane, 4.3 gm, 10.2 mM, 2 eq. was added to ten ml of 1,1,1,3 tetrachloroethane and the mixture stirred for several hours. A short path distillation head was added and the receiver flask was cooled in dry ice-acetone bath. The mixture was heated to 100° C. and the pressure lowered to 180 Ton. The desired product 3,3,3-Trifluoro-2-methyl-2-trifluoromethyl-propionaldehyde condensed in the receiver flask and was used without further purification in the above reaction. A short path distillation head was added the receiver flask was cooled in dry ice-acetone bath The desired product 3,3,3-Trifluoro-2-methyl-2-trifluoromethyl-propionaldehyde condensed in the receiver flask was used without further purification in the above reaction

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: In 4 ml of tetrahydrofuran was suspended 0.11 g of sodium hydride (60% in oil), to which 0.5 ml of a solution containing 0.44 g of 2,2-bis(trifluoromethyl)propanol in tetrahydrofuran was added dropwise at room temperature, followed by stirring for 10 minutes. To this was added dropwise 0.5 ml of a solution containing 0.3 g of 4,6-dichloropyrimidine in tetrahydrofuran at 0° C., followed by stirring at the same temperature for 1.5 hours. The reaction mixture was then poured into a saturated aqueous ammonium chloride solution, which was extracted three times with t-butyl methyl ether. The combined organic layers were washed with a saturated aqueous sodium chloride solution and dried over anhydrous magnesium sulfate to give a crude product of 4-chloro-6-[2,2-bis(trifluoromethyl)propoxy]pyrimidine. was added dropwise at room temperature by stirring at the same temperature for 1.5 hours was extracted three times with t-butyl methyl ether The combined organic layers were washed with a saturated aqueous sodium chloride solution dried over anhydrous magnesium sulfate

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: To 2,2-bis(trifluoromethyl)propanol (4.34 g, 22.1 mmol) in DCM (100 mL) at 0° C. add with stirring triethylamine (6.2 mL, 44 mmol) followed by methanesulfonyl chloride (2.6 mL, 33 mmol). After 15 min at 0° C. dilute with water and extract three times with EtOAc. Dry over anhydrous Na2SO4 and concentrate in vacuo to give the crude desired intermediate as a yellow oil (6.16 g, 100%). extract three times with EtOAc Dry over anhydrous Na2SO4 concentrate in vacuo