反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
To a solution of 3.5 g (13 mmol) of 4-(3-chloropropoxy)-benzenesulfonyl chloride in 100 ml of CH2Cl2, a solution of 1.62 g (18.56 mmol) of neopentyl amine in 15 ml of CH2Cl2 and 2.59 ml (18.56 mmol) of triethyl amine are added dropwise at 0–5° C. After stirring for 2.5 h at r.t., the reaction mixture is neutralized with 1 N aqueous HCl and extracted with AcOEt. The combined extracts are washed with brine, dried over MgSO4 and concentrated under reduced pressure to give 4-(3-chloropropoxy)-N-(2,2-dimethyl-propyl)-benzenesulfonamide; NMR (CDCl3): 0.879 (s, 9H), 2.20–2.35 (m, 2H), 2.66 (d, 2H, J=6.88 Hz), 3.76 (t, 2H, J=6.28 Hz), 4.20 (t, 2H, J=5.84 Hz), 4.35–4.465 (m, 1H), 6.98 (d, 2H, J=8.88 Hz), 7.77 (d, 2H, J=8.88 Hz).
WORKUP
后处理
- extractionextracted with AcOEt
- washThe combined extracts are washed with brine
- dry with materialdried over MgSO4
- concentrationconcentrated under reduced pressure