반응 #2066032

반응 방정식

trimethyl orthoformate

montmorillonite K10

3-(4-chloro-3-formylphenyl)-2,4-dioxo-1-methyl-6-trifluoromethyl-1,2,3,4-tetrahydropyrimidine

→

3-[4-Chloro-3-dimethoxymethylphenyl]-2,4-dioxo-1-methyl-6-trifluoromethyl-1,2,3,4-tetrahydropyrimidine

용매

toluene

반응 조건

후처리

1. 1
   온도while cooling with ice
2. 2
   workup.STIRRINGthe batch was stirred overnight at 25° C
3. 3
   여과The montmorillonite K10 was filtered off
4. 4
   세척washed thoroughly with toluene
5. 5
   workup.DISTILLATIONThe solvent, excess ortho-ester and methyl formate were distilled off under reduced pressure from the combined filtrates
6. 6
   기타The remaining oil was crystallized with petroleum ether

실험 절차

170 ml of trimethyl orthoformate were added to a thoroughly stirred suspension of 136 g of montmorillonite K10 in 700 ml of anhydrous toluene, and stirring was carried out for 30 minutes. Thereafter, 68.0 g of 3-(4-chloro-3-formylphenyl)-2,4-dioxo-1-methyl-6-trifluoromethyl-1,2,3,4-tetrahydropyrimidine were added dropwise while cooling with ice, and the batch was stirred overnight at 25° C. The montmorillonite K10 was filtered off and washed thoroughly with toluene. The solvent, excess ortho-ester and methyl formate were distilled off under reduced pressure from the combined filtrates. The remaining oil was crystallized with petroleum ether.

출처