HRID1823322

反应详情

EQUATION

反应方程式

HRID 1823322 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 2[(benzyloxy)methyl-8-methyl-2,3-dihydro[1,4]dioxino[2,3-f]quinoline (0.30 g, 0.94 mmol) in CH2Cl2 (8 mL) being cooled in an ice-bath, FeCl3 (0.77 g, 4.7 mmol) was added. After 1 h, the ice-bath was removed and the reaction mixture was stirred for another 4 h. CH2Cl2 (30 mL) and 1; N, NaOH (25 mL) were added to result in a suspension which was then filtered. The filtered solid was washed with CH3OH (50 mL). The combined organic layers were concentrated in vacuo. Purification on SiO2, eluted with (10:1) CHCl3:iPrOH gave 0.15 g (68%) of the title compound as an off-white solid.

WORKUP

后处理

  1. customthe ice-bath was removed
  2. additionN, NaOH (25 mL) were added
  3. customto result in a suspension which
  4. filtrationwas then filtered
  5. washThe filtered solid was washed with CH3OH (50 mL)
  6. concentrationThe combined organic layers were concentrated in vacuo
  7. customPurification on SiO2
  8. washeluted with (10:1) CHCl3