HRID480457

反应详情

EQUATION

反应方程式

HRID 480457 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

CONDITIONS

反应条件

温度
80 °C

PROCEDURE

实验过程

6-[1-hydroxy-2-methyl-1-(1-trityl-1H-imidazol-4-yl)propyl]-2-naphthyl trifluoromethanesulfonate (2.0 g), phenylboronic acid (446 mg), tetrakis(triphenylphosphine)-palladium (0) (115 mg) and lithium chloride (259 mg) were dissolved in dimethoxyethane (DME, 20 mL). Ag.Na2CO3 (2M, 4.5 mL) was added to the mixture, and whole was heated at 80° C. for 20 h. Water was added, the mixture was extracted with AcOEt. The extract was washed with brine, dried and concentrated. The residue was purified by column chromatography (eluent, hexane:THF=2:1) to give the titled compound (1.50 g) as a pale yellow powder.

WORKUP

后处理

  1. extractionthe mixture was extracted with AcOEt
  2. washThe extract was washed with brine
  3. customdried
  4. concentrationconcentrated
  5. customThe residue was purified by column chromatography (eluent, hexane:THF=2:1)