反应详情

A solution of methyl 4-pentylaminobenzoate (43) (200 mg, 0.91 mmole) in 5 mL of THF was treated with 95 mg of triphosgene (0.35 eq.), stirred at reflux for three hours, then poured onto 50 mL ice-water and extracted with three portions of 50 mL of ethyl acetate. The combined organic extracts were dried over MgSO4, filtered and concentrated in vacuo to give 250 mg of 4-methoxycarbonylphenyl-pentyl-carbamoyl chloride (45) which was used without purification.

1. temperatureat reflux for three hours
2. extractionextracted with three portions of 50 mL of ethyl acetate
3. dry with materialThe combined organic extracts were dried over MgSO4
4. filtrationfiltered
5. concentrationconcentrated in vacuo