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
N-(4-Amino-benzyl)-N′-cyano-N″-quinolin-5-yl-guanidine (133 mg, 0.50 mmol) and 9H-fluorene-9-carboxylic acid (105 mg, 0.50 mmol) were suspended in N,N-dimethylformamide(1.0 mL). Benzotriazol-1-yloxy-tris(dimethylamino)phosphonium hexafluorophosphate (232 mg, 0.52 mmol) was added followed by N,N-diisopropylethylamine (0.20 mL, 1.15 mmol). The reaction mixture was stirred at room temperature for 24 hours and then diluted with ethyl acetate (30 mL). This solution was washed with water (30 mL×2) and dried over anhydrous sodium sulfate. The solvent was removed in vacuo to give the desired product (102 mg, 44.5%). 1H NMR (DMSO-d6, ppm): 10.72 (s, 1H), 9.59 (bs, 1H), 8.37 (d, 2H), 8.27 (bs, 1H), 7.90 (d, 2H), 7.60 (t, 4H), 7.43 (t, 2H), 7.31 (m, 4H), 7.18 (m, 2H), 5.03 (s, 1H), 4.43 (d, 2H).
WORKUP
后处理
- washThis solution was washed with water (30 mL×2)
- dry with materialdried over anhydrous sodium sulfate
- customThe solvent was removed in vacuo