反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
CONDITIONS
反应条件
- 温度
- 40 °C
PROCEDURE
实验过程
1-(2,6-Dichloro-3,5-difluorophenyl)ethanol (133 mg, 0.586 mmol), 4-[4-(7-Hydroxy-6-nitrofuro[3,2-c]pyridin-3-yl)-pyrazol-1-yl]-piperidine-1-carboxylic acid tert-butyl ester (250 mg, 0.52 mmol), PPh3 (410 mg, 1.60 mmol) and THF (20 mL) was added to a dry round bottom flask. Diisopropyl azodicarboxylate (320 mg, 1.60 mmol) was added and the reaction mixture was heated at 40° C. More DIAD (320 mg, 1.60 mmol) was then added and the reaction mixture was heated at 40° C. for 2 h. Purification by flash column chromatography using 10%→40% EtOAc in hexanes afforded the title compound as a yellow solid. MS (ES+): m/z 581.88/583.80 (100/80) [MH+−isobutene]. HPLC: tR=4.29 min (ZQ3, polar—5 min).
WORKUP
后处理
- temperaturethe reaction mixture was heated at 40° C. for 2 h
- customPurification by flash column chromatography