HRID1669059

反应详情

EQUATION

反应方程式

HRID 1669059 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. temperatureThe mixture was cooled
  2. customthe solvent evaporated
  3. customthe residue purified by chromatography
  4. washeluting with 20% EtOAc/pet. ether