反应详情

A mixture of whole amount of 4-(3-chloro-4-methoxybenzylamino)-5-chloroformyl-6-chloro-2-methylthiopyrimidine (prepared in the above (1)), methylene chloride 15 ml and 2-benzyloxyethanol 224 mg is refluxed for 30 minutes. After cooling the reaction mixture is diluted with water and neutralized with an aqueous saturated sodium hydrogen carbonate solution. The solution is washed with ethyl acetate. The methylene chloride layer is diluted with ethyl acetate, washed, dried and concentrated in vacuo. The residue is separated with silica gel chromatography (solvent; hexane:ethyl acetate=5:1) to give 4-(3-chloro-4-methoxybenzylamino)-5-(2-benzyloxyethoxycarbonyl)-6-chloro-2-methylthiopyrimidine as a colorless oil 655 mg.

1. temperatureis refluxed for 30 minutes
2. temperatureAfter cooling the reaction mixture
3. washThe solution is washed with ethyl acetate
4. additionThe methylene chloride layer is diluted with ethyl acetate
5. washwashed
6. customdried
7. concentrationconcentrated in vacuo
8. customThe residue is separated with silica gel chromatography (solvent; hexane:ethyl acetate=5:1)