2,4-Dichloro-alpha-(chloromethyl)benzenemethanol methanesulfonate synthesis
- Product Name:2,4-Dichloro-alpha-(chloromethyl)benzenemethanol methanesulfonate
- CAS Number:53984-39-7
- Molecular formula:C9H9Cl3O3S
- Molecular Weight:303.59
Yield:53984-39-7 673 mg
Reaction Conditions:
with triethylamine in ethyl acetate at 0; for 0.166667 h;
Steps:
1.2 Preparation of [2-chloro-1-(2,4-dichlorophenyl)ethyllmethanesulfonate
A 10 mL flask is charged with 2-chloro-1-(2,4-dichlorophenyl)ethanol (0.5 g, 2.22 mmol), Et3N (347 pL, 2.44 mmol) and EtOAc (3 mL). The mixture is cooled at 0 °C with an ice bath and MsCl (174 μL, 2.22 mmol) is added dropwise. After 10 minutes at 0 °C, the resultingsuspension is filtered and quenched with H2O (10 mL). The aqueous phase is extracted with AcOEt (2 x 5 mL). The combined organic phases are washed with brine (5 mL), dried with Na2SO4, filtered and evaporated to give [2-chloro-1-(2,4-dichlorophenyl)ethyl]methanesulfonate as a light yellow oil (673 mg). 1H-NMR (400 MHz, CDCl3): δ= 7.52 (d, J = 8.4 Hz, 1 H), 7.44 (d, J = 2.0 Hz, 1 H), 7.36 (dd, J = 8.4, 2.0 Hz, 1 H), 6.06 (dd, J= 8.0, 3.7 Hz, 1H), 3.86 (dd, J= 12.2, 3.7 Hz, 1H), 3.75 (dd, J= 12.2, 8.0 Hz, 1H),3.09 (s, 3H).
References:
WO2015/3991,2015,A1 Location in patent:Page/Page column 41; 42
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