HRID456850

反应详情

EQUATION

反应方程式

HRID 456850 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 4-bromobenzoyl chloride (10.0 g) in dry dichloromethane (60 mL) at 0° C. was slowly added diisopropylamine (19 mL; 3.0 eq). The reaction was stirred overnight under nitrogen and gradually warmed to room temperature. The solution was washed with two portions of water and the organics were dried over anhydrous magnesium sulfate, filtered and concentrated. The residue was purified by flash chromatography eluting with 15% ethyl acetate. Near quantitative yield of product was obtained.

WORKUP

后处理

  1. customat 0° C.
  2. washThe solution was washed with two portions of water
  3. dry with materialthe organics were dried over anhydrous magnesium sulfate
  4. filtrationfiltered
  5. concentrationconcentrated
  6. customThe residue was purified by flash chromatography
  7. washeluting with 15% ethyl acetate