反应详情

温度

150 °C

A mixture of 6-bromo-chroman-3-ylamine (0.105 g, 0.46 mmol, 1 eq), (2S,5R)-4-(3-chloro-propyl)-2,5-dimethyl-piperazine-1-carboxylic acid tert-butyl ester (0.133 g, 0.46 mmol, 1 eq), K2CO3 (0.127 g, 0.92 mmol, 2 eq), and Kl (0.017 g, 0.10 mmol, 0.2 eq) in DMF (0.5 mL) was heated in a microwave reactor at 150° C. for 25 min. The reaction mixture was partitioned between EtOAc (3 mL) and 10% aqueous NaHCO3 (3 mL). The organic layer was separated and aqueous layer was extracted with EtOAc (2 mL×3). The combined organic layers were dried (Na2SO4) and concentrated in vacuo to give 0.22 g (100%) of (2S,5R)-4-[3-(6-bromo-chroman-3-ylamino)-propyl]-2,5-dimethyl-piperazine-1-carboxylic acid tert-butyl ester as a yellow oil. The material was carried on to next step without further purification.

1. customThe reaction mixture was partitioned between EtOAc (3 mL) and 10% aqueous NaHCO3 (3 mL)
2. customThe organic layer was separated
3. extractionaqueous layer was extracted with EtOAc (2 mL×3)
4. dry with materialThe combined organic layers were dried (Na2SO4)
5. concentrationconcentrated in vacuo