Methyl iodide → HCID 67165187, compound

Participants

Reaction Steps

A solution of Step 2 intermediate (5 g, 19.15 mmol) in dry DMF (56 ml) was added anhydrous K2CO3 (3.17 g, 22.98 mmol) and the mixture was stirred at room temperature for 30 min. Methyl iodide (1.43 ml, 22.98 mmol) was added drop-wise and the mixture was further stirred at room temperature for 24 h. The reaction mixture was diluted with water (100 ml) and the solid precipitated out was filtered and washed with water and dried to give 5.5 g of the product as off white solid; 1H NMR (δ ppm, DMSO-d6, 300 MHz): 7.90 (t, J=7.8, 1H); 7.66 (d, J=8.7, 1H); 7.55 (d, J=7.8, 1H); 3.76 (d, J=7.2, 2H); 3.55 (s, 3H); 1.20-1.10 (m, 1H); 0.47-0.40 (m, 2H); 0.35-0.28 (m, 2H).

Provenance & Evidence