反应详情

温度

0 °C

(2S,6RS)-4-[3-(Benzhydryl-amino)-4-cyano-benzyl]-2,6-dimethyl-3-oxo-piperazine-1-carboxylic acid benzyl ester (2.6 g, 5.21 mmol) is dissolved in 100 mL of ethyl acetate and cooled to 0° C. A 12N solution of hydrochloric acid (0.5 ml, 6.0 mmol) is added dropwise. The deprotection is complete in thirty minutes. The reaction mixture is washed with 10% sodium bicarbonate. The ethyl acetate layer is dried with magnesium sulfate, filtered and condensed. The resulting residue is purified by flash colunm (SiO2, 60% ethyl acetate/hexane) to give the product (2S,6RS)-4-(3-amino)-4-cyano-benzyl)-2,6-dimethyl-3-oxo-piperazine-1-carboxylic acid benzyl ester (2.03 g, 99%).

1. waitThe deprotection is complete in thirty minutes
2. washThe reaction mixture is washed with 10% sodium bicarbonate
3. dry with materialThe ethyl acetate layer is dried with magnesium sulfate
4. filtrationfiltered
5. customcondensed
6. customThe resulting residue is purified by flash colunm (SiO2, 60% ethyl acetate/hexane)