ChemicalBook CAS DataBase List 2-[2-(2,2,2-Trifluoroethoxy)phenoxy]ethyl methanesulfonate

2-[2-(2,2,2-Trifluoroethoxy)phenoxy]ethyl methanesulfonate synthesis

9synthesis methods

Product Name:2-[2-(2,2,2-Trifluoroethoxy)phenoxy]ethyl methanesulfonate
CAS Number:160969-03-9
Molecular formula:C11H13F3O5S
Molecular Weight:314.28

Anhydrous AlCl3 ( 165 g, 1 .24 mol) and 200 mL of anhydrous dichloromethane were mixed, cooled to -5 ℃ under nitrogen protection, methane sulfonyl chloride was added dropwise with stirring, and then stirred at room temperature for 30 min after the dropwis

124-63-0
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2-[2-(2,2,2-Trifluoroethoxy)phenoxy]ethanol

160969-02-8
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2-[2-(2,2,2-Trifluoroethoxy)phenoxy]ethyl methanesulfonate

160969-03-9
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Yield:160969-03-9 92.5%

Reaction Conditions:

with triethylamine in dichloromethane at 0 - 20; for 4 h;Reflux;

Steps:

1.4; 2.4; 3.4; 4.4 S4,Synthesis of 2-[2-(2,2,2-trifluoroethoxy)phenoxy]ethyl methanesulfonate (Formula I)
In a 5000 mL four-necked flask equipped with mechanical stirring, 200 g (0.85 mol, 1.0 eq) of 2-[2-(2,2,2-trifluoroethoxy)phenoxy]ethyl alcohol which was involved in the reaction was sequentially added. ,The temperature of the reaction system was lowered to about 0 ° C under 155 g (1.53 mol, 1.8 eq) of triethylamine and 2400 ml of ice cream in dichloromethane.388 g (3.4 mol, 4.0 eq) of methanesulfonyl chloride dissolved in 1000 ml of dichloromethane was slowly added dropwise.The temperature of the reaction system was controlled to be not higher than 20 °C. After the addition is completed, remove the ice salt bath.The temperature was raised to reflux for 4 hours, cooled to room temperature, and triethylamine hydrochloride was removed by filtration.The filtrate was washed with 1000 ml of *3 saturated sodium carbonate.Dry over anhydrous sodium sulfate, filter, dry EtOAc m.400 g of isopropanol was added and stirred at 0 ° C for 6 hours, and filtered.Vacuum drying to 247 g of a white solid.Melting point 39-42 ° C,The yield is 92.5%.The purity is 98.3%.

References:

Anhui Qingyun Pharmaceutical Co., Ltd.;Huang Huan;Huang Qingguo;Li Kai;Shi Yaqin CN109516933, 2019, A Location in patent:Paragraph 0043; 0051-0053; 0061-0063 0071-0073; 0081-0082

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