反应详情

2′,4′-Dichlorobiphenyl-4-sulfonic acid-(3-hydroxymethyl-phenyl)-amide (ABD455) (0.4 g) was dissolved in DMF (20 ml). K2CO3 (1 g) was added followed by methyl iodide (1 ml). The mixture was stirred vigorously for 3 hrs, poured into water and extracted with ether. After drying (Na2SO4), the solvent was partially removed under vacuum and petrol added to induce crystallisation and the product collected as white crystals. 13C NMR (CDCl3): δ 38.4, 64.7, 125.3, 125.7, 126.0, 127.5, 127.7, 129.2, 129.8, 130.1, 131.9, 133.1, 134.9, 135.8, 137.2, 141.6, 142.0 and 142.8. 1H NMR (CDCl3): δ 3.22 (3H, s), 4.65 (2H, d, J=5.8 Hz), 7.02 (1H, m), 7.14 (1H, s), 7.28 (1H, s), 7.30 (3H, m), 7.48 (2H, d, J=8.2 Hz), 7.50 (1H, m) and 7.60 (2H, d, J=8.2 Hz).

1. extractionextracted with ether
2. dry with materialAfter drying (Na2SO4)
3. customthe solvent was partially removed under vacuum and petrol
4. additionadded
5. customcrystallisation
6. customthe product collected as white crystals