反应详情

温度

0 °C

To a solution of 6-methoxy-α-methyl-2-naphthalenacetic acid (4.02 g, 17.5 mmoles) in toluene (30 ml) and N,N-dimethylformamide (0.3 ml) cooled at 0° C., oxalylchloride (2.92 ml, 34.06 mmoles) is added. After 2 hours at room temperature, the solution is evaporated at reduced pressure. The obtained residue is dissolved in acetone (50 ml) and the solution is added to a solution of 4-thiazolidincarboxylic acid (2.33 g, 17.5 mmoles) and triethylamine (6.34 ml, 45.5 mmoles) in acetone (50 ml) cooled at 0° C. After 2 hours the solution is acidified with HCl 4 N, concentrated under vacuum, the residue is treated with ethyl acetate and the organic phase is washed first with HCl 2 N, then with water. The organic phase is anhydrified with sodium sulphate and evaporated at reduced pressure. 4.43 g of the expected product are obtained in the form of a white solid having m.p. 165° C.-168° C.

1. customthe solution is evaporated at reduced pressure
2. dissolutionThe obtained residue is dissolved in acetone (50 ml)
3. concentrationconcentrated under vacuum
4. additionthe residue is treated with ethyl acetate
5. washthe organic phase is washed first with HCl 2 N
6. customevaporated at reduced pressure