반응 #520890

반응 방정식

2,5-difluoro-4-[3-methyl-2,6-dioxo-4-(trifluoromethyl)-1,2,3,6-tetrahydropyrimidin-1-yl]nitrobenzene

sodium hydride

3-benzyloxyphenol

→

2-(3-benzyloxyphenoxy)-5-fluoro-4-[3-methyl-2,6-dioxo-4-(trifluoromethyl)-1,2,3,6-tetrahydropyrimidin-1-yl]nitrobenzene

수율 52.9%

용매

N,N-dimethylformamide

N,N-dimethylformamide

N,N-dimethylformamide

반응 조건

후처리

1. 1
   온도while cooling with ice
2. 2
   workup.ADDITIONwas added dropwise at the same temperature
3. 3
   workup.STIRRINGstirred for 1 hour
4. 4
   추출extracted with ethyl acetate
5. 5
   세척The organic layer was washed once with 1N hydrochloric acid and once with saturated saline
6. 6
   건조dried over anhydrous magnesium sulfate
7. 7
   농축concentrated

실험 절차

A mixture of 1.71 g of 3-benzyloxyphenol and 4.0 ml of N,N-dimethylformamide was added dropwise into a mixture of 0.34 g of sodium hydride and 8.5 ml of N,N-dimethylformamide while cooling with ice, and the mixture was stirred for 20 minutes. A mixture of 3.0 g of 2,5-difluoro-4-[3-methyl-2,6-dioxo-4-(trifluoromethyl)-1,2,3,6-tetrahydropyrimidin-1-yl]nitrobenzene (described later, produced in Intermediate Production Example 4) and 7.0 ml of N,N-dimethylformamide was added dropwise at the same temperature, and stirred for 1 hour. This reaction solution was poured into ice water, and extracted with ethyl acetate. The organic layer was washed once with 1N hydrochloric acid and once with saturated saline, and dried over anhydrous magnesium sulfate, and concentrated. The residue was subjected to silica gel column chromatography to obtain 2.4 g of 2-(3-benzyloxyphenoxy)-5-fluoro-4-[3-methyl-2,6-dioxo-4-(trifluoromethyl)-1,2,3,6-tetrahydropyrimidin-1-yl]nitrobenzene.

출처