反应 #657257

ord-852f47be86574ff68e08c58c5bd293f0

反应方程式

CCOCc1cnn(C(c2ccccc2)(c2ccccc2)c2ccccc2)c1
1-trityl-4-ethoxymethylpyrazole
CCOCc1cn[nH]c1
4-ethoxymethylpyrazole
收率 44.0%

反应条件

温度
80°CELSIUS
详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    workup.ADDITIONwas added to the resulting solution
  2. 2
    温度After cooling to room temperature
  3. 3
    过滤the reaction mixture was filtered
  4. 4
    洗涤washed with dichloromethane
  5. 5
    萃取extracted with dichloromethane
  6. 6
    干燥dried over MgSO4
  7. 7
    其他the solvent was evaporated under vacuum

实验过程

1-trityl-4-ethoxymethylpyrazole (1.800 g, 4.88 mmol) was dissolved in a mixture of ethanol/acetone (15 ml/5 ml) and 30 mL of 2N HCl was added to the resulting solution. The mixture was heated at 80° C. for 2 h. After cooling to room temperature, the reaction mixture was filtered and washed with dichloromethane. The aqueous layer was basified with 2N NaOH and extracted with dichloromethane. The organic layers were combined, dried over MgSO4 and the solvent was evaporated under vacuum yielding compound 4-ethoxymethylpyrazole as a white oil. Yield: 44% (270 mg, 2.14 mmol).

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US09023315B2uspto-grants-2015_05