HRID625483

反应详情

EQUATION

反应方程式

HRID 625483 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 3-iodobenzoic acid (9.92 g, 40.00 mmol, 1.00 equiv) in DMF (100 mL), 1-(bromomethyl)benzene (6.84 g, 40.00 mmol, 1.00 equiv), potassium carbonate (11.04 g, 80.00 mmol, 2.00 equiv). The resulting solution was stirred for 2 h at room temperature. The solids were filtered out and the filtrate was concentrated under vacuum. The residue was diluted with 50 mL of water and extracted with 2×50 mL of ethyl acetate. The combined organic layers were washed with 2×50 mL of sodium chloride, dried over anhydrous sodium sulfate and concentrated under vacuum to give 13.1 g (97%) of benzyl 3-iodobenzoate as light brown oil

WORKUP

后处理

  1. customInto a 500-mL round-bottom flask, was placed
  2. filtrationThe solids were filtered out
  3. concentrationthe filtrate was concentrated under vacuum
  4. additionThe residue was diluted with 50 mL of water
  5. extractionextracted with 2×50 mL of ethyl acetate
  6. washThe combined organic layers were washed with 2×50 mL of sodium chloride
  7. dry with materialdried over anhydrous sodium sulfate
  8. concentrationconcentrated under vacuum