反应详情

A solution of 384 mg of 4-cyano-3-methoxyphenyl isocyanate (prepared according to WO 2007/137874) in 8 mL dioxane is added to a solution of 200 mg of 2-hydroxymethyl-2-phenylglycine (prepared according to literature procedure) in an aqueous solution of 1.8 mL 1N sodium hydroxide in 2 mL of water. The mixture is stirred at room temperature overnight, acidified by adding 3 mL 12N HCl and heated at 110° C. for 2 hours. The solution is then treated with a saturated aqueous solution of sodium bicarbonate, extracted with ethyl acetate, dried over sulfate magnesium, filtered, evaporated and purified over silica gel while eluting with 60/40 heptane/ethyl acetate mixture to give the expected product.

1. temperatureheated at 110° C. for 2 hours
2. extractionextracted with ethyl acetate
3. dry with materialdried over sulfate magnesium
4. filtrationfiltered
5. customevaporated
6. custompurified over silica gel
7. washwhile eluting with 60/40 heptane/ethyl acetate mixture