HRID55000

反应详情

EQUATION

反应方程式

HRID 55000 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

A mixture of 4-bromopyridine (40.6 g, 0.25 mmol), palladium acetate (1.16 g, 5.14 mmol), tri-(O-tolyl)phosphine (3.14 g, 10.3 mmol), CH3CN (129 mL), triethylamine (64.3 mL, 0.46 mmol) and methyl acrylate (46.8 mL, 0.514 mmol) was sealed in a bomb and placed in an oil bath at 120° C. for 4 hours. The mixture was cooled to 0° C., the bomb was vented, and the slurry thus obtained was partitioned between CH2Cl2 /water. The aqueous phase was separated, extracted with CH2Cl2 (2×200 mL) and the combined organic layers were dried over MgSO4. The solvent was removed in vacuo to afford 38 g of methyl 3-(4-pyridyl)propenoate.

WORKUP

后处理

  1. customwas sealed in a bomb
  2. customthe slurry thus obtained
  3. customwas partitioned between CH2Cl2 /water
  4. customThe aqueous phase was separated
  5. extractionextracted with CH2Cl2 (2×200 mL)
  6. dry with materialthe combined organic layers were dried over MgSO4
  7. customThe solvent was removed in vacuo