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
CONDITIONS
反应条件
- 温度
- 40 °C
PROCEDURE
实验过程
To 25 mL of DMSO was added 4.5 g of 5-bromo-4-chloro-5,6,7,8-tetrahydro-2-trifluoromethylquinazoline and 4.7 g of anhydrous sodium acetate. The reaction mixture was warmed for 2 hours at which time 4.1 g of N-[[2'-(1H-tetrazol-5-yl)[1,1'-biphenyl]-4-yl]methyl]amine hydrochloride was added and the reaction was heated to 40° C. overnight. The crude reaction mixture was purified on silica gel (20% methanol/chloroform) to yield the title product (1.9 g, 24%); 1H NMR (DMSO-d6, 400 MHz) δ 7.78 (m, 1H), 7.63 (m, 2H), 7.53 (m, 2H), 7.24 (m, 2H); 7.03 (m, 2H), 5.64 (m, 1H), 4.52 (m,2H), 2.68 (m, 2H), 2.23 (m, 1H), 1.97 (s, 3H), 1.80 (m, 3H); positive DCI MS m/e 510 (M+H). Anal. calcd for C25H22F3N7O2 : C, 58.94; H, 4.35; N, 19.24. Found: C, 58.31; H, 4.30; N, 19.20.
WORKUP
后处理
- additionwas added
- customThe crude reaction mixture
- customwas purified on silica gel (20% methanol/chloroform)