反应详情

tert-Butyl 3-[(cyclopropylmethoxy)methyl]pyrrolidine-1-carboxylate (Preparation 66, 50 g, 0.2 mol, 1 eq) was dissolved in isopropanol (200 mL) and treated with concentrated hydrogen chloride solution (28 mL, 0.3 mol, 1.5 eq). The mixture was refluxed for 1 h and evaporated. The residue was dissolved in water and washed with ether (2×100 mL). The aqueous fraction was made alkaline with potassium carbonate to pH 12-13 and extracted with chloroform. The extract was dried over sodium sulfate and evaporated to give title compound (20 g, 0.129 mol, 65%).

1. temperatureThe mixture was refluxed for 1 h
2. customevaporated
3. dissolutionThe residue was dissolved in water
4. washwashed with ether (2×100 mL)
5. extractionextracted with chloroform
6. dry with materialThe extract was dried over sodium sulfate
7. customevaporated