HRID1669059
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
- 85 °C
PROCEDURE
实验过程
Alternative Preparation of Ethyl-7,8-dihydro-6H-indeno[5,6-e][1,2,4]triazine 1-Oxide (67). Pd(dppf)Cl2 (130 mg, 0.08 mmol) was added under N2 to a N2-purged solution of chloride 21 (350 mg, 1.6 mmol) and SnEt4 (455 mg, 1.9 mmol) in DME (20 mL) and the mixture was stirred at 85° C. for 16 h. The mixture was cooled, the solvent evaporated and the residue purified by chromatography, eluting with 20% EtOAc/pet. ether, to give (i) starting material 21 (148 mg, 42%) and (ii) 1-oxide 67 (84 mg, 25%) as a yellow solid: mp 79-81° C., spectroscopically identical to the sample prepared above.
WORKUP
后处理
- temperatureThe mixture was cooled
- customthe solvent evaporated
- customthe residue purified by chromatography
- washeluting with 20% EtOAc/pet. ether