HRID30615

反应详情

EQUATION

反应方程式

HRID 30615 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A stirred solution of [2-(4-bromo-2-[1,3]dioxan-2-yl-phenoxy)-ethyl]-dimethyl-amine (15 mmol) in dry THF (100 mL) was cooled to −78° C. and added n-BuLi (16.5 mmol) dropwise. The reaction was left for 30 min at −78° C. and added triisopropyl borate (22.5 mmol). The reaction was heated to room temperature, was added 2M HCl (aq, 50 mL) and was left for an additional, hour. The mixture was added 1M Na2CO3 to neutral pH and was extracted with EtOAc. The organic phase was washed with water, dried (Na2SO4) and evaporated in vacuo. Addition of EtOAc afforded beige crystals that was filtered of and was used without further purification.

WORKUP

后处理

  1. waitwas left for an additional, hour
  2. extractionwas extracted with EtOAc
  3. washThe organic phase was washed with water
  4. dry with materialdried (Na2SO4)
  5. customevaporated in vacuo
  6. additionAddition of EtOAc afforded beige crystals that
  7. filtrationwas filtered of and
  8. customwas used without further purification