反应 #2328996

反应方程式

tert-Butyl [5-(6-methoxy-1,3-benzoxazol-2-yl)pyridin-2-yl]carbamate

sodium hydride

sodium hydride

1-bromo-2-fluoroethane

1-bromo-2-fluoroethane

→

tert-butyl (2-fluoroethyl)[5-(6-methoxy-1,3-benzoxazol-2-yl)pyridin-2-yl]carbamate

溶剂

DMF

反应条件

后处理

1. 1
   其他The solvent was removed under reduced pressure
2. 2
   workup.DISSOLUTIONredissolved in EtOAc
3. 3
   workup.ADDITIONWater was added
4. 4
   其他the layers separated
5. 5
   萃取The aqueous layer was extracted with EtOAc (2×)
6. 6
   干燥dried (Na2SO4)
7. 7
   其他evaporated
8. 8
   其他to give 253 mg as brown oil
9. 9
   其他The crude product was taken to the next step without further purification

实验过程

tert-Butyl [5-(6-methoxy-1,3-benzoxazol-2-yl)pyridin-2-yl]carbamate (0.65 mmol) and sodium hydride (0.78 mmol) were dissolved in dry DMF (20 mL) at 0° C. After 5 min 1-bromo-2-fluoroethane (0.72 mmol) was added and the reaction was allowed to warm to r.t. After 2 h additional sodium hydride and 1-bromo-2-fluoroethane was added and the reaction mixture was stirred over night. The solvent was removed under reduced pressure and redissolved in EtOAc. Water was added and the layers separated. The aqueous layer was extracted with EtOAc (2×), dried (Na2SO4) and evaporated to give 253 mg as brown oil. The crude product was taken to the next step without further purification. MS m/z 388 (M+H).

来源