反应详情

Into 30 mL of 50% aqueous methanol, was dissolved 1.76 g (20 mmoles) of 1,4-butanediamine followed by the addition of 5.48 g (20 mmoles) of S-benzyloxycarbonyl-4,6-dimethyl-2-mercaptopyrimidine (a product of Kokusan Kagaku Co.). The mixture was stirred for 3 hours. Thereafter, the reaction mixture was filtered to remove the precipitated di-N-benzyloxycarbonyl compound [2.09 g (29%) were recovered], and the filtrate was evaporated to dryness. The residue was dissolved in 250 mL of chloroform, washed 5 times with 100 mL of water. The chloroform layer was dried over anhydrous sodium sulfate, and evaporated to dryness to obtain 1.0 g (23% yield) of mono-N-benzyloxycarbonyl-1,4-butanediamine in colorless syrup form.

1. filtrationThereafter, the reaction mixture was filtered
2. customto remove the precipitated di-N-benzyloxycarbonyl compound [2.09 g (29%) were recovered]
3. customthe filtrate was evaporated to dryness
4. dissolutionThe residue was dissolved in 250 mL of chloroform
5. washwashed 5 times with 100 mL of water
6. dry with materialThe chloroform layer was dried over anhydrous sodium sulfate
7. customevaporated to dryness