HRID2097464

反应详情

EQUATION

反应方程式

HRID 2097464 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To 7.26 g (25.3 mmol) of 4-bromo-2-cyclobutoxy-1-methoxymethoxybenzene obtained in Reference Example 5-(c) was added 30 ml of 1,4-dioxane solution containing 4N hydrogen chloride, and the mixture was stirred at room temperature for 24 hours. After completion of the reaction, 100 ml of water was added to the reaction mixture, and the mixture was extracted with diethyl ether. The organic layer after separation was washed with a saturated aqueous solution of sodium chloride, dried over anhydrous sodium sulfate and then concentrated under reduced pressure. The obtained residue was applied to silica gel column chromatography (Eluent; hexane:ethyl acetate=9:1 (V/V)), and the fractions containing the desired compound were concentrated under reduced pressure to obtain 3.07 g of the title compound as a pale yellowish oil. (Yield: 50%)

WORKUP

后处理

  1. additionwas added to the reaction mixture
  2. extractionthe mixture was extracted with diethyl ether
  3. customThe organic layer after separation
  4. washwas washed with a saturated aqueous solution of sodium chloride
  5. dry with materialdried over anhydrous sodium sulfate
  6. concentrationconcentrated under reduced pressure
  7. additionthe fractions containing the desired compound
  8. concentrationwere concentrated under reduced pressure