HRID63860

反应详情

EQUATION

反应方程式

HRID 63860 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Into a 500-mL round-bottom flask, was placed a solution of methyl 4-bromo-3-methylbenzoate (10 g, 43.65 mmol, 1.00 equiv) in CCl4 (150 ml), NBS (8.12 g, 45.62 mmol, 1.05 equiv). The resulting solution was heated to reflux overnight under 100 w incandescent bulb. The solids were filtered out. The resulting mixture was concentrated under vacuum. The residue was applied onto a silica gel column with ethyl acetate/petroleum ether (1:30-1:10). This resulted in 6 g (47%) of methyl 4-bromo-3-(bromomethyl)benzoate as a off-white solid.

WORKUP

后处理

  1. customInto a 500-mL round-bottom flask, was placed
  2. temperatureThe resulting solution was heated
  3. temperatureto reflux overnight under 100 w incandescent bulb
  4. filtrationThe solids were filtered out
  5. concentrationThe resulting mixture was concentrated under vacuum
  6. customThis resulted in 6 g (47%) of methyl 4-bromo-3-(bromomethyl)benzoate as a off-white solid