HRID2224093
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
- 135 °C
PROCEDURE
实验过程
N-Benzyl-3-(butyrylamino)thiophene-2-carboxamide (1-4, 2.00 g, 6.60 mmol) was dissolved in ethylene glycol (15.0 mL) and treated with NaOH pellets (26 mg, 0.66 mmol). The reaction was heated to 135° C. for 3 h and allowed to cool. The reaction was diluted with EtOAc (100 mL) and washed with NH4Cl, H2O (2×20 mL), NaCl (30 mL) and dried with MgSO4. Organics were concentrated to provide 3-benzyl-2-propylthieno[3,2-d]pyrimidin-4(3H)-one (1-5). 1H NMR (300 MHz, CDCl3) δ7.77 (d, J=5.2 Hz, 1H), 7.30 (m, 4H), 7.17 (d, J=6.4 Hz, 2H), 5.43 (s, 2H), 2.73 (m, 2H), 1.85 (m, 2H), 0.98 (t, J=7.3 Hz, 3H); MS 285.0 found 284.3 required.
WORKUP
后处理
- temperatureto cool
- washwashed with NH4Cl, H2O (2×20 mL), NaCl (30 mL)
- dry with materialdried with MgSO4
- concentrationOrganics were concentrated