反应详情

A mixture of (2R,3R,4R)-3,4-dibenzyloxy-2-benzyloxymethylpyrrolidine (Compound 1) (0.5 g, 1.24 mmol), formic acid (10 ml) and 37% formaldehyde (7.5 ml) was heated for 3 hours at reflux temperature and evaporated in vacuo. The residue was dissolved in a mixture of ethyl acetate (25 ml) and 1 N sodium hydroxide (25 ml). The organic phase was isolated, washed once with water, dried over magnesium sulphate and evaporated in vacuo to give (2R,3R,4R)-3,4-dibenzyloxy-2-benzyloxymethyl-1-methylpyrrolidine (0.49 g, yield: 95%) as a golden oil.

1. temperaturewas heated for 3 hours
2. temperatureat reflux temperature
3. customevaporated in vacuo
4. dissolutionThe residue was dissolved in a mixture of ethyl acetate (25 ml) and 1 N sodium hydroxide (25 ml)
5. customThe organic phase was isolated
6. washwashed once with water
7. dry with materialdried over magnesium sulphate
8. customevaporated in vacuo