反応 #982184

反応方程式

1,3-dimethyl-2-oxabicyclo[2,2,2]octan-5,6-dione-5-oxime-6-hydrazone

trimethylorthobenzoate

→

3-phenyl-5,8-dihydro-6,8-dimethyl-5,8-ethano-6H-pyrano[4,3-e]-as-triazine-4-oxide

反応条件

後処理

1. 1
   その他is removed
2. 2
   温度The resulting mixture is cooled
3. 3
   その他evaporated to dryness in vacuo
4. 4
   ろ過After filtering the residue
5. 5
   workup.DISSOLUTIONdissolved in 2% methanol-chloroform through silica gel, and evaporation of the filtrate

実験手順

A solution of 1.97 g. (0.01 mole) 1,3-dimethyl-2-oxabicyclo[2,2,2]octan-5,6-dione-5-oxime-6-hydrazone in 10 ml. trimethylorthobenzoate is refluxed under nitrogen for 18 hours at a bath temperature of 140° C. during which time all distillate is removed. The resulting mixture is cooled and evaporated to dryness in vacuo. After filtering the residue dissolved in 2% methanol-chloroform through silica gel, and evaporation of the filtrate gives 3-phenyl-5,8-dihydro-6,8-dimethyl-5,8-ethano-6H-pyrano[4,3-e]-as-triazine-4-oxide.

出典