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3,6-Dimethoxy-9H-fluoren-9-one synthesis

11synthesis methods
-

Yield:13235-07-9 90%

Reaction Conditions:

with bis(trifluoromethyl sulfate)palladium;tert-butylisonitrile;water;silver carbonate in dimethyl sulfoxide at 140; for 24 h;Reagent/catalyst;

Steps:

3. Synthesis of 3

General procedure: A mixture of 1 (0.5 mmol),DMSO (50% aq, 3 mL), Pd(OTf)2 (5 mol%), Ag2CO3 (2equiv) was stirred at 140°C under air atmosphere for 24 h. The reaction mixture was washed water and the aqueous phase was extracted with ethyl acetate (3 times). The combined organic layer was washed with brine, dried over Na2SO4, and evaporated under reduced pressure. The crude product was purified by silica gel column chromatography to give the corresponding products. (3a-3i1, 3k-3m1, 3o-3p1, according to the literature)

References:

Cai, Zhiqiang;Hou, Xu;Hou, Ling;Hu, Zhiquan;Zhang, Bo;Jin, Zhengsheng [Synlett,2016,vol. 27,# 3,art. no. ST-2015-W0682-L,p. 395 - 398] Location in patent:supporting information