反应详情

A solution of 1.65 g (4.59 mmol) of 1-benzyl-7-benzyloxy-3-hydroxymethyl-2-methylpyrrolo [2,3-d]pyridazine, 3.8 g (18.6 mmol) of dicyclohexylcarbodiimide and 1.6 ml (27.4 mmol) of glacial acetic acid in 50 ml of anhydrous tetrahydrofuran is stirred at room temperature for 18 h. The solution is then treated with 50 ml of water, rendered neutral with saturated sodiumhydrogen carbonate solution and extracted with 3×50 ml of dichloromethane. The organic extracts are washed with 50 ml of water, dried over magnesium sulfate and concentrated. The residue which remains is chromatographed on silica gel (eluent: ethyl acetate). After crystallization from diisopropyl ether, 1.3 g (71%) of the title compound are isolated. M.p.: 121°-122° C.

1. extractionextracted with 3×50 ml of dichloromethane
2. washThe organic extracts are washed with 50 ml of water
3. dry with materialdried over magnesium sulfate
4. concentrationconcentrated
5. customThe residue which remains is chromatographed on silica gel (eluent: ethyl acetate)
6. customAfter crystallization from diisopropyl ether, 1.3 g (71%) of the title compound
7. customare isolated