Triethylamine → 2-(Dimethoxymethyl)-3-(methoxymethoxy)-4-(trifluoromethyl)benzyl methanesulfonate

Triethylamine (2.74 ml, 19.7 mmol) was added to a solution of [2-(dimethoxymethyl)-3-(methoxymethoxy)-4-(trifluoromethyl)phenyl]methanol (5.09 g, 16.4 mmol) obtained in Example (6-6) in ethyl acetate (50 ml). After methanesulfonyl chloride (1.33 ml, 17.2 mmol) was added dropwise to the mixture under ice-cooling, the reaction mixture was stirred at the same temperature for 30 minutes. The reaction mixture was filtered through Celite. The filtrate was successively washed with a saturated aqueous sodium hydrogencarbonate solution, water and a saturated aqueous NaCl solution and dried with anhydrous sodium sulfate. n-Hexane was added to the residue obtained by removing the solvent under reduced pressure. The precipitated crystals were filtered to give 2-(dimethoxymethyl)-3-(methoxymethoxy)-4-(trifluoromethyl)benzyl methanesulfonate as a pale yellow compound (5.37 g, yield: 84%).

1. temperaturecooling
2. filtrationThe reaction mixture was filtered through Celite
3. washThe filtrate was successively washed with a saturated aqueous sodium hydrogencarbonate solution, water
4. dry with materiala saturated aqueous NaCl solution and dried with anhydrous sodium sulfate
5. additionn-Hexane was added to the residue
6. customobtained
7. customby removing the solvent under reduced pressure
8. filtrationThe precipitated crystals were filtered

ORD-Eintrag

ord-68e2d28eaa1740aeac428db8951a1641

Quelldatensatz

uspto-grants-2011_04

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US07923573B2