반응 #214334

반응 방정식

p-anisidine

2-methyl-2-hydroxy-butan-3-one

acetic acid

toluene

→

5-methoxy-2,3,3-trimethyl-indolenine

용매

water

water

반응 조건

후처리

1. 1
   workup.DISTILLATIONThe solvent is then distilled off
2. 2
   온도After cooling to 160° C.
3. 3
   workup.ADDITION10 parts of concentrated sulfuric acid are added
4. 4
   workup.DISTILLATIONwhilst distilling off the water
5. 5
   기타formed
6. 6
   workup.DISTILLATIONDistillation under reduced pressure (21 mbar)

실험 절차

246 parts of p-anisidine, 204 parts of 2-methyl-2-hydroxy-butan-3-one and 10 parts of acetic acid in 650 parts of toluene are heated, with removal of water from the system, until no more water separates off. The solvent is then distilled off and the residue is heated for 5 hours at 220° C. After cooling to 160° C., 10 parts of concentrated sulfuric acid are added; the mixture is kept at 160° C. for 3 hours, whilst distilling off the water formed. Distillation under reduced pressure (21 mbar) gives 318.7 parts of 5-methoxy-2,3,3-trimethyl-indolenine (melting point 53°-54° C.), corresponding to 84.3% of theory.

출처