反应详情

温度

60 °C

A 7 mL vial was charged with 4-(3-chloropropyl)-4H-benzo[1,4]oxazin-3-one (1.0 equiv), K2CO3 (2.0 equiv), NaI (2.0 equiv) and 4-Butylpiperidine (1.05 equiv) in 5 mL dry MeCN and shaken at 60° C. for 48 h. The reaction mixture was evaporated to dryness, diluted with 10 mL H2O, extracted into CH2Cl2 (3×13 mL), and filtered through a PTFF Whatman filter. The combined organic layers were evaporated to dryness and purified by CC (Heptane/EtOAc or CH2Cl2/MeOH) or prep TLC (Heptane/EtOAc or CH2Cl2/MeOH).

1. customThe reaction mixture was evaporated to dryness
2. additiondiluted with 10 mL H2O
3. extractionextracted into CH2Cl2 (3×13 mL)
4. filtrationfiltered through a PTFF Whatman
5. filtrationfilter
6. customThe combined organic layers were evaporated to dryness
7. custompurified by CC (Heptane/EtOAc or CH2Cl2/MeOH) or prep TLC (Heptane/EtOAc or CH2Cl2/MeOH)