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6,8-Dichloro-2H-chromen-2-one synthesis

5synthesis methods
-

Yield:20300-61-2 80%

Reaction Conditions:

with polyphosphoric acid in N,N-dimethyl-formamide at 145; for 4 h;Inert atmosphere;

Steps:

2. General procedure for the preparation of coumarins 3 (3a-3j)

General procedure: To the solution of polyphosphoric acid (PPA, 0.6 mmol) in DMF (0.3 mL) were added salicylaldehydes 1 (0.3 mmol) and acetic anhydride 2 (1.2 mmol) under a nitrogen atmosphere. The reaction mixture was stirred at 145°C 3-6 h. The reaction mixture was quenched with water and extracted with ethyl acetate. The organic layer was washed with saturated sodium bicarbonate solution, dried over Na2SO4 and evaporated. The resulting crude compound was purified by silica gel column chromatography, affording the pure coumarins 3.

References:

Yang, Li-Shou;Wang, Yu;Wang, En-Hua;Yang, Jan;Pan, Xiong;Liao, Xiu;Yang, Xiao-Sheng [Synthetic Communications,2020,p. 1 - 6] Location in patent:supporting information