HRID355604

反应详情

EQUATION

反应方程式

HRID 355604 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 1,3,3-trimethyl-2-methyleneindoline (0.435 g; 0.0025 mol) and 2-hydroxy-1-nitroso-4-piperidinodibenzofuran (0.675 g; 0.0025 mol) in methanol (25.0 ml) was heated under nitrogen and refluxed with stirring for 41 hours. The solution was evaporated to dryness and chromatographed over silica (eluent: dichloromethane) to yield 1,3,3-trimethyl-6'-piperidinospiro[2H-indole 2,3'-[3H]-[2H-[1,4]benzoxazino [6,5-b]benzofuran]] as an amber oil (0.35 g; 32%), which afforded a pale yellow solid upon trituration with diethyl ether, m.pt. 213.5°-216° C.; λmaxAbsorbance 570 nm (Polyurethane). ##STR13##

WORKUP

后处理

  1. temperaturewas heated under nitrogen
  2. temperaturerefluxed
  3. customThe solution was evaporated to dryness
  4. customchromatographed over silica (eluent: dichloromethane)