반응 #64226

반응 방정식

sodium hydride

water

sodium hydride

product

4-(4,4-dimethyl 2,5-dioxo 3-(4-hydroxy butyl) 1-imidazolidinyl) 2-(trifluoromethyl) benzonitrile

methyl iodide

methyl iodide

→

expected product

4-[4,4-dimethyl 2,5-dioxo 3-(4-methoxybutyl) 1-imidazolidinyl] 2-(trifluoromethyl)-benzonitrile

용매

dimethylformamide

반응 조건

후처리

1. 1
   workup.STIRRINGthe mixture was stirred for one hour
2. 2
   workup.WAITafter 20 minutes
3. 3
   추출extracted with ether
4. 4
   세척The extracts were washed with water
5. 5
   기타dried
6. 6
   기타the solvent was evaporated
7. 7
   기타The residue was chromatographed on silica (eluant: methylene chloride--acetone 98-2)

실험 절차

50 mg of sodium hydride were added in several lots to 370 mg of the product of Example 58 in solution in 3 ml of dimethylformamide and the mixture was stirred for 20 minutes. 0.06 ml of methyl iodide were added and the mixture was stirred for one hour. A further 50 mg of sodium hydride were added and then after 20 minutes, 0.06 ml of methyl iodide were added. The reaction medium was poured into water and extracted with ether. The extracts were washed with water, dried and the solvent was evaporated. The residue was chromatographed on silica (eluant: methylene chloride--acetone 98-2) to obtain 135 mg of the expected product melting at 80°-81° C.

출처