HRID402142

反应详情

EQUATION

反应方程式

HRID 402142 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of (2-amino-4-methoxy-3-methylphenyl)(methyl)ketone (18.6 g, 104 mmol) in dioxane (50 mL) was added under nitrogen to a suspension of 4-isopropylthiazole-2-carbonyl chloride in dioxane (250 mL). After 2 h at room temperature, the reaction mixture was concentrated to dryness. Then, the residue was partitioned between an aqueous solution of NaHCO3 and AcOEt, organic layer was washed with brine, dried (Na2SO4), and evaporated. The residue was triturated in diisopropyl ether, filtered off and washed with diisopropyl ether to give 30.8 g (90%) of the title product 35.

WORKUP

后处理

  1. concentrationthe reaction mixture was concentrated to dryness
  2. customThen, the residue was partitioned between an aqueous solution of NaHCO3 and AcOEt, organic layer
  3. washwas washed with brine
  4. dry with materialdried (Na2SO4)
  5. customevaporated
  6. customThe residue was triturated in diisopropyl ether
  7. filtrationfiltered off
  8. washwashed with diisopropyl ether