反应详情

2.18 g (0.0102 mmole) (3RS)-3-(N-tertbutyloxycarbonylaminoethyl) pyrrolidine and 2.81 g (0.0125 mole) N-benzyloxycarbonyl-S-methylisothiourea was dissolved in 30 ml toluene and heated to 60°-70° C. for eight hours followed by stirring at room temperature for one day. 0.3M KHSO4 -solution was added and the water layer was washed with a mixture of the toluene and ethyl acetate and left for 2 days under which time the Boc group was removed. The acidic water phase was made alkaline and extracted four times with CH2Cl2. The combined organic layer was dried (Na2SO4), filtered and evaporated to yield 2.0 g (51%) of the title compound.

1. temperatureheated to 60°-70° C. for eight hours
2. washthe water layer was washed with a mixture of the toluene and ethyl acetate
3. waitleft for 2 days under which time the Boc group
4. customwas removed
5. extractionextracted four times with CH2Cl2
6. dry with materialThe combined organic layer was dried (Na2SO4)
7. filtrationfiltered
8. customevaporated