反应详情

With stirring, 10.1 g of 1-{1-[2-hydroxy-3-(3-chloropyrazin-2-yloxy)-propyl]-4-piperidinyl}-3-phenyl-imidazolidin-2-one (see Example 6) and 1.41 g of sodium methylate in 110 ml of methanol are refluxed for 10 hours. The reaction mixture is concentrated in a water jet vacuum. The residue is dissolved in ethyl acetate and extracted with 2N hydrochloric acid. The combined hydrochloric acid extracts are made alkaline with conc. ammonia and extracted with methylene chloride. The combined methylene chloride extracts are washed with water, dried over sodium sulphate and concentrated in a water jet vacuum. The residue crystallises from methylene chloride-ether to yield 1-{1-[2-hydroxy-3-(3-methoxy-pyrazin-2-yloxy)-propyl]-4-piperidinyl} -3-phenyl-imidazolidin-2-one with a melting point of 128°-129° C.

1. concentrationThe reaction mixture is concentrated in a water jet vacuum
2. dissolutionThe residue is dissolved in ethyl acetate
3. extractionextracted with 2N hydrochloric acid
4. extractionextracted with methylene chloride
5. washThe combined methylene chloride extracts are washed with water
6. dry with materialdried over sodium sulphate
7. concentrationconcentrated in a water jet vacuum
8. customThe residue crystallises from methylene chloride-ether