反应详情

A mixture of 2.5 g (10 mmol) of (E)-3-[2-[4-(cyclopropyl)-2-thiazolyl]ethenyl]benzeneamine prepared as in example 1 as above, 1.5 g (15 mol) of succinic anhydride, 1.64 g (20 mmol) of anhydrous sodium acetate and 200 ml of 1,2-dimethoxyethane was stirred and heated under reflux for 2 hr. The reaction mixture was cooled and concentrated in vacuo. The residue was heated on the steam bath with 200 ml of water for 0.5 hr. The solid was collected and recrystallized from ethanol to give 1.4 g of (E)-4-[[3-[2-(4-cyclopropyl-2-thiazolyl)-ethenyl]phenyl]amino]-4-oxobutanoic acid, mp 177°-179° dec, as off-white needles.

1. temperatureheated
2. temperatureunder reflux for 2 hr
3. temperatureThe reaction mixture was cooled
4. concentrationconcentrated in vacuo
5. temperatureThe residue was heated on the steam bath with 200 ml of water for 0.5 hr
6. customThe solid was collected
7. customrecrystallized from ethanol