HRID71051

反应详情

EQUATION

反应方程式

HRID 71051 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
-78 °C

PROCEDURE

实验过程

To a solution of 1,2-diiodo-3,5-dimethylbenzene (0.5 g, 1.40 mmol) in 60 mL in a mixture of THF and Et2O (1:1), was added dropwise at −78° C. isopropylmagnesium chloride (2 M in THF, 0.70 mL, 1.40 mmol). After the mixture was stirred for 2 h at −78° C., B(OiPr)3 (0.96 ml, 4.19 mmol) was added. The solution was warmed to room temperature overnight, then a saturated solution of NH4Cl was added, and the resulting mixture was stirred for 30 min at room temperature. The aqueous layer was extracted with Et2O (50 mL, 3 times), dried over Na2SO4 and concentrated. To the concentrated sample, hexane was added and the resulting precipitate was isolated to provide the products as shown above as non separable mixture.

WORKUP

后处理

  1. temperatureThe solution was warmed to room temperature overnight
  2. stirringthe resulting mixture was stirred for 30 min at room temperature
  3. extractionThe aqueous layer was extracted with Et2O (50 mL, 3 times)
  4. dry with materialdried over Na2SO4
  5. concentrationconcentrated
  6. additionTo the concentrated sample, hexane was added
  7. customthe resulting precipitate was isolated
  8. customto provide the products