HRID1773967

反应详情

EQUATION

反应方程式

HRID 1773967 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 5-bromo-2-chlorophenol (2.08 g, 10 mmol, 1.0 eq.) and potassium carbonate (4.15 g, 30 mmol, 3.0 eq.) in MeCN (19 mL), 2-iodopropane (1.53 mL, 15 mmol, 1.5 eq.) was added. The mixture was stirred at r.t. for 18 hours. The mixture was heated up to 50° C. and stirred at that temperature for 2.5 hours. The reaction mixture was partitioned between AcOEt and water. The layers were separated and the aq. phase was extracted with AcOEt (2×). The comb. org. extracts were washed with water and sat. aq. NaCl soln., dried over MgSO4, filtered, and concentrated in vacuo to give 4-bromo-1-chloro-2-isopropoxy-benzene as a yellow oil. The product was used without further purification. LC-MS 3: tR=0.98 min; [M+H]+=no ionization

WORKUP

后处理

  1. temperatureThe mixture was heated up to 50° C.
  2. stirringstirred at that temperature for 2.5 hours
  3. customThe reaction mixture was partitioned between AcOEt and water
  4. customThe layers were separated
  5. extractionthe aq. phase was extracted with AcOEt (2×)
  6. washextracts were washed with water and sat. aq. NaCl soln
  7. dry with material, dried over MgSO4
  8. filtrationfiltered
  9. concentrationconcentrated in vacuo