HRID220484

反应详情

EQUATION

反应方程式

HRID 220484 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
130 °C

PROCEDURE

实验过程

Dissolve 1H-pyrazole-4-carboxaldehyde in N,N-dimethylformamide (1.9 mL). Add potassium carbonate (0.539 g, 3.90 mmol) and cyclopropylbromide (0.346 g, 2.86 mmol). Heat in a pressure tube to 130° C. for 18 hr. Cool to ambient temperature and add DCM and water. Separate layers and extract water layer 3 times with DCM. Wash combined DCM layers with brine, dry (magnesium sulfate), filter, and concentrated to give the free base of the title preparation. GC-MS: m/z=136 [M+].

WORKUP

后处理

  1. temperatureCool to ambient temperature
  2. extractionSeparate layers and extract water layer 3 times with DCM
  3. washWash
  4. dry with materialdry (magnesium sulfate)
  5. filtrationfilter
  6. concentrationconcentrated
  7. customto give the free base of the title
  8. custompreparation