HRID68609

反应详情

EQUATION

反应方程式

HRID 68609 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a cooled solution (0° C.) of 3-(4-fluoro-3-(methylsulfonyl)phenyl)-4-methoxybenzaldehyde (27) (400 mg, 1.3 mmol, 1 eq.) in DCM (20 mL) was added BBr3 (0.4 mL). The reaction mixture was stirred room temperature for 3 h. After cooling to 0° C., methanol was added and the mixture was concentrated under vacuum. The residue was diluted with DCM and washed with water. The DCM was dried (Na2SO4) and concentrated in vacuo. The residue was purified by column chromatography (eluent: PE:EA=1:1) to give 340 mg (89%) of 3-(4-fluoro-3-(methylsulfonyl)phenyl)-4-hydroxybenzaldehyde (28).

WORKUP

后处理

  1. temperatureAfter cooling to 0° C.
  2. concentrationthe mixture was concentrated under vacuum
  3. additionThe residue was diluted with DCM
  4. washwashed with water
  5. dry with materialThe DCM was dried (Na2SO4)
  6. concentrationconcentrated in vacuo
  7. customThe residue was purified by column chromatography (eluent: PE:EA=1:1)