HRID446359

反应详情

EQUATION

反应方程式

HRID 446359 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Dibenzoyl peroxide (0.5 g) was added to a stirred mixture of 2-(3-fluoro-5-methylphenyl)acetic acid (5.95 g) and NBS (6.93 g) in dichloromethane (120 mL). The resultant mixture was heated at reflux for 5 hours. The reaction mixture was cooled to room temperature and then washed twice with water. The organic layer was dried, filtered and the solvent concentrated under reduced pressure. The crude product was purified by flash silica chromatography using 1% acetic acid and 17% ethyl acetate in isohexane as solvent. Fractions containing the product were concentrated to dryness to afford the subtitled compound. Yield 6.50 g.

WORKUP

后处理

  1. temperatureat reflux for 5 hours
  2. washwashed twice with water
  3. customThe organic layer was dried
  4. filtrationfiltered
  5. concentrationthe solvent concentrated under reduced pressure
  6. customThe crude product was purified by flash silica chromatography
  7. additionFractions containing the product
  8. concentrationwere concentrated to dryness