Potassium Carbonate → HCID 68539007, compound

Participants

Reaction Conditions

Reaction Steps

A mixture of compound 25 (200 mg, 0.5 mmol), K2CO3 (420 mg, 3.0 mmol) and phenyltrimethyl ammonium chloride (254 mg, 1.5 mmol) and 50 ml water-free N,N-dimethylformamide was stirred for 9 h at 80° C. (bath temperature) under N2. After filtration from the inorganic residue, the filtrate was evaporated down, and the evaporation residue was purified using column chromatography (silica gel; CH2Cl2/MeOH/conc. NH4OH (93:7:1)). The evaporation residue (250 mg of foamy resin) was dissolved in MeOH and salicylic acid added to it. 102 mg (41%) of the compound 26.C7H6O3 was isolated. Fp. 110-115° C.; IR (KBr): 1720 (CO) cm−1; 1H-NMR (CDCl3): δ 7.29-7.18 (m, 5 arom. H), 6.75, (s, 2 arom. H), 3.93 (s, C4—OCH3), 3.80 (s, C3—OCH3), 2.31 (s, NCH3); MS (CI): m/z 450 (M++1).

Provenance & Evidence