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
The solution of tert-butyl (4-(2-(3-methyl-1H-1,2,4-triazol-1-yl)-5-nitrophenoxy)butyl)carbamate (515 mg, 1.316 mmol) in CH2Cl2 (4 mL) was treated with TFA (2 mL, 26.0 mmol) at 0° C. The mixture was stirred at rt for 2 h. The reaction mixture was concentrated in vacuo and the residue was triturated with ether to yield a white solid, which was collected by filtration to get 4-(2-(3-methyl-1H-1,2,4-triazol-1-yl)-5-nitrophenoxy)butan-1-amine, TFA (440 mg, 83% yield). LC-MS (M+H)+=292.4. 1H NMR (500 MHz, methanol-d4) δ 8.99 (s, 1H), 8.11 (d, J=1.5 Hz, 1H), 8.05 (dd, J=2.1, 1.3 Hz, 2H), 4.38 (t, J=6.2 Hz, 2H), 3.07-2.94 (m, 2H), 2.48 (s, 3H), 2.02 (dd, J=8.8, 6.3 Hz, 2H), 1.84 (d, J=7.5 Hz, 2H).
WORKUP
后处理
- concentrationThe reaction mixture was concentrated in vacuo
- customthe residue was triturated with ether
- customto yield a white solid, which
- filtrationwas collected by filtration