反応 #4427

反応方程式

3,4-dihydro-6-(3,4-dimethoxyphenyl)-3-methyl-2-(1-piperazinyl)-4-(2,4,6-trimethylphenylimino)pyrimidine

triethylamine

4-fluorobenzoyl chloride

→

3,4-dihydro-6-(3,4-dimethoxyphenyl)-2-[4-(4-fluorobenzoyl)piperazin-1-yl]-3-methyl-4-(2,4,6-trimethylphenylimino)pyrimidine

溶媒

tetrahydrofuran

反応条件

後処理

1. 1
   その他the reaction was quenched
2. 2
   workup.ADDITIONby adding methanol (5 ml)
3. 3
   その他After evaporation of the solvent
4. 4
   workup.DISSOLUTIONthe residue was dissolved in ethyl acetate
5. 5
   洗浄The solution was washed with water
6. 6
   乾燥dried over magnesium sulfate
7. 7
   その他evaporated in vacuo
8. 8
   その他The residue was chromatographed on silica gel using
9. 9
   workup.ADDITIONa mixture of chloroform and methanol (95:5)

実験手順

To a suspension of 3,4-dihydro-6-(3,4-dimethoxyphenyl)-3-methyl-2-(1-piperazinyl)-4-(2,4,6-trimethylphenylimino)pyrimidine (0.31 g) in tetrahydrofuran (10 ml) were added triethylamine (0.11 ml) and 4-fluorobenzoyl chloride (0.69 ml). The mixture was stirred at ambient temperature for an hour and the reaction was quenched by adding methanol (5 ml). After evaporation of the solvent, the residue was dissolved in ethyl acetate. The solution was washed with water, dried over magnesium sulfate and evaporated in vacuo. The residue was chromatographed on silica gel using a mixture of chloroform and methanol (95:5) to give 3,4-dihydro-6-(3,4-dimethoxyphenyl)-2-[4-(4-fluorobenzoyl)piperazin-1-yl]-3-methyl-4-(2,4,6-trimethylphenylimino)pyrimidine (0.34 g).

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