反応 #2358566

ord-89befef5af27451b9069002b35f0c443

反応方程式

COc1ccc(S(=O)(=O)Cl)cc1OC
3,4-dimethoxybenzenesulfonyl chloride
CCN(CC)CC
triethylamine
CCCCCCN
hexylamine
CCCCCCNS(=O)(=O)c1ccc(OC)c(OC)c1
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. 1
    ろ過The reaction mixture was filtered
  2. 2
    洗浄the filtrate was washed 1N HCl (2×)
  3. 3
    乾燥dried with MgSO4
  4. 4
    ろ過filtered
  5. 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).

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US09120744B2uspto-grants-2015_09