HRID1097771

反应详情

EQUATION

反应方程式

HRID 1097771 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

1-Methoxy-1-(trimethylsiloxy)-2-methyl-1-propene (2.4 mL, 2.092 g, 12 mmol) is added dropwise to a suspension of 2-Nitro-benzaldehyde (1.51 g, 10 mmol), Scandium (III) trifluoromethanesulfonate (148 mg, 0.3 mmol) in 30 mL of dry CH2Cl2 at −78° C. The resulting mixture is slowly warmed up to 0° C. and stirred for 1 h. The reaction is quenched with 1 M HCl and stirred for 1 h at room temperature. After extraction with ethyl acetate (20 mL×3), washed with brine, dried over anhydrous Na2SO4 and concentration, the residue is purified by flash column, and gives a yellow oil (800 mg).

WORKUP

后处理

  1. customThe reaction is quenched with 1 M HCl
  2. stirringstirred for 1 h at room temperature
  3. extractionAfter extraction with ethyl acetate (20 mL×3)
  4. washwashed with brine
  5. dry with materialdried over anhydrous Na2SO4 and concentration
  6. customthe residue is purified by flash column