反应详情

A solution of 20 g. 4-[14-(trimethylsilyl)tetradecylamino]benzoyl chloride hydrochloride in 100 ml. dioxane is added to 4.9 g. freshly prepared ethyl glycinate in 300 ml. of methylene chloride containing 1 g. of 4-(dimethylamino)pyridine and 10 ml. of triethylamine. After 16 hours at room temperature the reaction is refluxed for 2 hours, cooled and filtered. The mother liquor is extracted with water and 10% hydrochloric acid. The solution is dried and concentrated in vacuo to an amber liquid. A sample is chromatographed on silica, appropriate fractions are pooled and evaporated to yield a solid which is recrystallized to a white solid.

1. temperaturecooled
2. filtrationfiltered
3. extractionThe mother liquor is extracted with water and 10% hydrochloric acid
4. customThe solution is dried
5. concentrationconcentrated in vacuo to an amber liquid
6. customA sample is chromatographed on silica, appropriate fractions
7. customevaporated
8. customto yield a solid which
9. customis recrystallized to a white solid