反応 #4422

反応方程式

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

→

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

収率 26.3%

溶媒

ethanol

反応条件

後処理

1. 1
   その他After removal of the catalist
2. 2
   ろ過by filtration
3. 3
   その他the filtrate was evaporated in vacuo
4. 4
   抽出extracted with ethyl acetate
5. 5
   乾燥The extract was dried over magnesium sulfate
6. 6
   その他evaporated in vacuo
7. 7
   その他The residue was chromatographed on silica gel
8. 8
   workup.ADDITIONThe fractions containing the desired compound
9. 9
   その他evaporated in vacuo
10. 10
    その他to give a residue, which
11. 11
    その他was recrystallized from ethyl acetate

実験手順

To a suspension of 2-chloro-3,4-dihydro-6-(3,4-dimethoxyphenyl)-3-methyl-4-(2,4,6-trimethylphenylimino)pyrimidine (1.5 g) in ethanol (20 ml) was added 10%-palladium on carbon (0.8 g). The mixture was stirred under hydrogen (1 atm) for 40 minutes. After removal of the catalist by filtration, the filtrate was evaporated in vacuo. The residue was neutralized with aqueous sodium bicarbonate and extracted with ethyl acetate. The extract was dried over magnesium sulfate and evaporated in vacuo. The residue was chromatographed on silica gel using chloroform. The fractions containing the desired compound were combined and evaporated in vacuo to give a residue, which was recrystallized from ethyl acetate to afford 3,4-dihydro-6-(3,4-dimethoxyphenyl)-3-methyl-4-(2,4,6-trimethylphenylimino)pyrimidine (0.36 g).

出典