HRID1371030

反应详情

EQUATION

反应方程式

HRID 1371030 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of the product from Step 1 (1.0 g, 3.7 mmol) and cinnamyl bromide (0.72 g, 3.7 mmol) in DMF (15 mL) at 0° C. under N2 was added the NaH (121 mg, 4.0 mmol, 80% in oil). After 20 min. at 0° C., the reaction was stirred for 1 h at r.t. Saturated NH4Cl (15 mL) was then added and the product was extracted with Et2O. The organic phase was washed with H2O and brine, and was then dried (MgSO4) filtered, and evaporated. The residue was purified by flash chromatography (1:10 EtOAc:hexane) to give a colourless oil (1.26 g).

WORKUP

后处理

  1. extractionthe product was extracted with Et2O
  2. washThe organic phase was washed with H2O and brine
  3. dry with materialwas then dried (MgSO4)
  4. filtrationfiltered
  5. customevaporated
  6. customThe residue was purified by flash chromatography (1:10 EtOAc:hexane)