HRID625207

反应详情

EQUATION

反应方程式

HRID 625207 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Into a 250-mL round-bottom flask, was placed a solution of 3-(bromomethyl)benzoic acid (7 g, 32.56 mmol, 1.00 equiv) in ethanol (80 mL), and potassium ethanethioate (9.65 g, 84.65 mmol, 2.60 equiv). The resulting solution was stirred overnight at room temperature. The resulting mixture was concentrated under vacuum. The resulting solution was diluted with 80 mL of water and adjusted to pH 3-4 with 10% hydrochloric acid. The resulting solution was extracted with 3×50 mL of ethyl acetate and the organic layers combined. The resulting mixture was washed with 1×50 mL of brine. The mixture was dried over sodium sulfate and concentrated under vacuum. This resulted in 4.4 g (64%) of 3-(acetylthiomethyl)benzoic acid as a brown solid.

WORKUP

后处理

  1. customInto a 250-mL round-bottom flask, was placed
  2. concentrationThe resulting mixture was concentrated under vacuum
  3. additionThe resulting solution was diluted with 80 mL of water
  4. extractionThe resulting solution was extracted with 3×50 mL of ethyl acetate
  5. washThe resulting mixture was washed with 1×50 mL of brine
  6. dry with materialThe mixture was dried over sodium sulfate
  7. concentrationconcentrated under vacuum
  8. customThis resulted in 4.4 g (64%) of 3-(acetylthiomethyl)benzoic acid as a brown solid