反応 #2358566
ord-89befef5af27451b9069002b35f0c443
反応方程式
3,4-dimethoxybenzenesulfonyl chloride
triethylamine
hexylamine
→
N-hexyl-3,4-dimethoxybenzenesulfonamide
収率 75.5%
反応条件
詳細条件
See reaction.notes.procedure_details.
後処理
- 1ろ過The reaction mixture was filtered
- 2洗浄the filtrate was washed 1N HCl (2×)
- 3乾燥dried with MgSO4
- 4ろ過filtered
- 5濃縮concentrated in vacuo
実験手順
To a solution of 3,4-dimethoxybenzenesulfonyl chloride (0.500 g, 2.11 mmol), triethylamine (0.750 mL, 5.30 mmol) in 7 mL of ethyl acetate, hexylamine (0.280 mL, 2.11 mmol) was added dropwise and the resulting solution was stirred overnight. The reaction mixture was filtered and the filtrate was washed 1N HCl (2×), dried with MgSO4, filtered and concentrated in vacuo to afford 0.480 g (75%) of N-hexyl-3,4-dimethoxybenzenesulfonamide as a white solid. 1H NMR (CDCl3, 400 MHz) δ 7.46 (m, 1H), 7.32 (m, 1H), 6.94 (m, 1H), 4.22 (m, 1H), 3.93 (s, 3H), 3.92 (s, 3H), 2.93 (q, J=6.4 Hz, 2H), 1.44 (quintet, J=6.9 Hz, 2H), 1.25 (m, 6H), 0.84 (t, J=6.9 Hz, 3H).