反应详情

温度

0 °C

0.7 g (2.53 mmole) (3RS)-1-(N-benzyloxycarbonylamidino)-3-hydroxymethylpyrrolidine and 0.70 ml (5.05 mmole) triethylamine was dissolved in 15 ml diethyl ether/CH2Cl2 1/1 and the mixture was cooled to 0° C. 0.25 ml (3.29 mole) methanesulphonyl chloride in 3 ml diethyl ether was slowly added and the reaction mixture was stirred at 0° C. for three hours. The solvent was evaporated and the residue was dissolved in ethyl acetate and extracted with a 0.3 M KHSO4-solution. The water layer was washed once with CH2Cl2 The water layer was made neutral with 10M NaOH-solution and extracted twice with CH2Cl2. The combined organic layer was dried (Na2SO4), filtered and evaporated to yield 0.450 g (50%) of the title compound.

1. customThe solvent was evaporated
2. dissolutionthe residue was dissolved in ethyl acetate
3. extractionextracted with a 0.3 M KHSO4-solution
4. washThe water layer was washed once with CH2Cl2 The water layer
5. extractionextracted twice with CH2Cl2
6. dry with materialThe combined organic layer was dried (Na2SO4)
7. filtrationfiltered
8. customevaporated