反应详情

In N,N-dimethylformamide (100 ml), N-tert-butoxycarbonylglycine (2.00 g), morpholine (1.00 ml), 1-hydroxybenzotriazole monohydrate (1.74 g) and 1-(dimethylaminopropyl)-3-ethylcarbodiimide hydrochloride (2.84 g) were dissolved, followed by stirring overnight at room temperature. After concentration under reduced pressure, the residue was diluted with dichloromethane, washed with water and dried over anhydrous sodium sulfate. The residue obtained by distilling off the solvent under reduced pressure was purified by chromatography on a silica gel column (dichloromethane:methanol=100:1), whereby a colorless foam was obtained. The substance was dissolved in dichloromethane (2 ml), followed by the addition of saturated solution of hydrochloride in ethanol (10 ml). The resulting mixture was stirred at room temperature for 5 minutes. The reaction mixture was concentrated to dryness under reduced pressure, whereby the title compound (1.80 g, quant.) was obtained as a pale yellow foam was obtained.

1. concentrationAfter concentration under reduced pressure
2. additionthe residue was diluted with dichloromethane
3. washwashed with water
4. dry with materialdried over anhydrous sodium sulfate
5. customThe residue obtained
6. distillationby distilling off the solvent under reduced pressure
7. customwas purified by chromatography on a silica gel column (dichloromethane:methanol=100:1), whereby a colorless foam
8. customwas obtained
9. stirringThe resulting mixture was stirred at room temperature for 5 minutes
10. concentrationThe reaction mixture was concentrated to dryness under reduced pressure, whereby the title compound (1.80 g, quant.)
11. customwas obtained as a pale yellow foam
12. customwas obtained