反应详情

温度

0 °C

To a mixture of 1-tert-Butoxycarbonylmethyl-pyrrolidine-3-carboxylic acid, Lithium salt (0.5 g, 2.12 mmol) and HOBt (0.45 g, 3.3 mmol) in DMF (10 ml) at 0° C. was added EDCl (630 mg, 3.3 mmol). The formed reaction mixture was stirred at 0° C. for 0.5 hour and then 4-amino-2-chloro-phenol was added. After stirred at RT for overnight, the reaction mixture was added to ice-water (50 g) and the formed precipitated was collected by filtration, washed with sodium bicarbonate and HCl (0.1 N). After drying in air, the crude product (720 mg) was used directly in the next step. Mass Spec ES (355.2, M+H)

1. customThe formed reaction mixture
2. stirringAfter stirred at RT for overnight
3. customthe formed precipitated
4. filtrationwas collected by filtration
5. washwashed with sodium bicarbonate and HCl (0.1 N)
6. customAfter drying in air