反应详情

To a solution of N2-methyl-N-[3-(triphenylphosphonio)propyl]glycinamide chloride (7.65 g, 17.9 mmol) in N,N-dimethylformamide (15 mL) was added 1-H-pyrazole-1-carboximidamide hydrochloride (2.76 g, 18.8 mmol) and N,N-diisopropylethylamine (3.28 mL, 18.8 mmol). The mixture was stirred overnight at room temperature. After stirring overnight, the reaction was not complete, and additional 1-H-pyrazole-1-carboximidamide hydrochloride (394 mg, 2.69 mmol) and N,N-diisopropylethylamine (0.47 mL, 2.69 mmol) were added. After 8 hours, additional 1-H-pyrazole-1-carboximidamide hydrochloride (338 mg, 2.3 mmol) and N,N-Diisopropylethylamine (0.40 mL, 2.3 mmol) were added again. The mixture was stirred overnight again. The reaction was diluted with methylene chloride (30 mL), and then the solution was added to a flask containing a rapidly stirring mixture of methylene chloride (15 mL) and methyl t-butyl ether (61 mL) to precipitate the product. The supernatant was decanted, and the product was dried under high vacuum at 35° C. to give the title compound (9.4 g, 100% yield about 80% pure) as a crude light yellow solid.

1. stirringAfter stirring overnight
2. waitAfter 8 hours
3. stirringThe mixture was stirred overnight again
4. additionthe solution was added to a flask
5. additioncontaining
6. stirringa rapidly stirring
7. customto precipitate the product
8. customThe supernatant was decanted
9. customthe product was dried under high vacuum at 35° C.