HRID1476362

反应详情

EQUATION

反应方程式

HRID 1476362 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A THF solution of n-decyl magnesium bromide (prepared as a THF (2 ml) solution of n-decyl bromide (2.2 ml, 11 mmol) and Mg (292 mg, 12 mmol)) was added to 6-bromo-2-methoxynaphthalene (2.37 g, 10 mmol) easily available from a reagent manufacturer and a THF (10 ml) solution of Ni(dppp)Cl2 (271 mg, 0.5 mmol), and the mixture was heated under reflux for 19 hours. After cooling, the mixed solution was diluted with water (10 ml), and non-reacted Mg was filtered out. The filtered solution was extracted with ether (5 ml×3). The extracted organic phases were collected (10 ml×3), and dried with MgSO4, and condensed with an evaporator. The condensed organic phase was recrystallized with hexane to obtain 6-n-decyl-2-methoxynaphthalene (compound (3)-64) as a light yellow solid.

WORKUP

后处理

  1. temperatureunder reflux for 19 hours
  2. temperatureAfter cooling
  3. filtrationwas filtered out
  4. extractionThe filtered solution was extracted with ether (5 ml×3)
  5. customThe extracted organic phases were collected (10 ml×3)
  6. dry with materialdried with MgSO4, and condensed with an evaporator
  7. customThe condensed organic phase was recrystallized with hexane