HRID579860

反应详情

EQUATION

反应方程式

HRID 579860 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To 36 ml of toluene were added 1.0 g (5.9/1000 mole) of 3-chloro-4-isopropylaniline and 0.7 g of pyridine, and 0.9 g (5.9/1000 mole) of 2-methylvaleryl chloride was added. The mixture was stirred at room temperature for 20 minutes. The crystals that precipitated were separated by filtration. Water (70 ml) was added to the filtrate, and the mixture was extracted with toluene. The toluene solution was washed with a saturated aqueous solution of sodium hydrogen carbonate, and dried over anhydrous sodium sulfate. The resulting dried solution was concentrated by an evaporator. Recrystallization of the resulting crude crystals from methanol gave 1.2 g of N-(3-chloro-4-isopropylphenyl)-2-methylvaleramide in a yield of 76.0 % based on 3-chloro-4-isopropylaniline.

WORKUP

后处理

  1. additionwas added
  2. customThe crystals that precipitated
  3. customwere separated by filtration
  4. additionWater (70 ml) was added to the filtrate
  5. extractionthe mixture was extracted with toluene
  6. washThe toluene solution was washed with a saturated aqueous solution of sodium hydrogen carbonate
  7. dry with materialdried over anhydrous sodium sulfate
  8. concentrationThe resulting dried solution was concentrated by an evaporator
  9. customRecrystallization of the resulting crude crystals from methanol