反应详情

2-Chloro-5-cyanopyridine (500 mg, 3.6 mmol), tert-butyl (2-mercaptoethyl)carbamate (426 mg, 2.4 mmol) and 1,8-diazabicyclo(5.4.0)undec-7-ene (549 mg, 3.6 mmol) are dissolved in DMF (5 ml) and stirred at RT under argon for 12 h. The reaction mixture is diluted with water (100 ml) and extracted with ethyl acetate (3×75 ml). The combined organic phases are washed with saturated aqueous sodium chloride solution, dried over magnesium sulphate and concentrated. After removal of the solvent, the residue is purified by preparative RP-HPLC (gradient of eluent: water/acetonitrile 90:10 to 10:90). 612 mg (91% of theory) of the product are obtained as a solid.

1. extractionextracted with ethyl acetate (3×75 ml)
2. washThe combined organic phases are washed with saturated aqueous sodium chloride solution
3. dry with materialdried over magnesium sulphate
4. concentrationconcentrated
5. customAfter removal of the solvent
6. customthe residue is purified by preparative RP-HPLC (gradient of eluent: water/acetonitrile 90:10 to 10:90)
7. custom612 mg (91% of theory) of the product are obtained as a solid