反应详情

温度

-78 °C

To a solution of 1.70 g (5.64 mmol) of 2-methyl-propane-2-sulfinic acid 1-(8-ethyl-1,4-dioxa-spiro[4.5]dec-8-yl)methylideneamide (prepared from 8-ethyl-1,4-dioxa-spiro[4.5]decane-8-carbonitrile using the protocol described for the synthesis of 19) and 982 mg (5.64 mmol) of fluoromethyl-phenyl sulfone in 60 mL of abs. tetrahydrofuran were added at −78° C. 5.92 mL (5.92 mmol) of a 1M solution of lithiumbis(trimethylsilyl)amide in tetrahydrofuran. The mixture was stirred for 1 h at −78° C. before being quenched by addition of saturated aqueous ammonium chloride solution and extracted twice with 100 mL of ethyl acetate. The combined organic layers were dried over magnesium sulphate, filtered, and concentrated in vacuo to give 2.65 g of the crude title compound. Rt=0.91 min (Method P). Detected mass: 476.4 (M+H+)

1. custombefore being quenched by addition of saturated aqueous ammonium chloride solution
2. extractionextracted twice with 100 mL of ethyl acetate
3. dry with materialThe combined organic layers were dried over magnesium sulphate
4. filtrationfiltered
5. concentrationconcentrated in vacuo