반응 #990798

반응 방정식

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

trimethylorthobenzoate

→

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

반응 조건

후처리

1. 1
   기타is removed
2. 2
   온도The resulting mixture is cooled
3. 3
   기타evaporated to dryness in vacuo
4. 4
   여과After filtering the residue
5. 5
   workup.DISSOLUTIONdissolved in 2% methanol-chloroform through silica gel, and evaporation of the filtrate the resulting solid
6. 6
   기타is triturated with ether

실험 절차

A solution of 2.11 g. (0.01 mole) 1,3,3-trimethyl-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 the resulting solid is triturated with ether, giving 3-phenyl-5,8-dihydro-6,6,8-trimethyl-5,8-ethano-6H-pyrano [4,3-e]-as-triazine-4-oxide; m.p. 186.5° to 189° C.

출처