HRID1415909

反应详情

EQUATION

反应方程式

HRID 1415909 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A mixture of tetrakis(triphenyl-phosphine)palladium (155 mg), 3-[5-(tert-butyldimethylsilyloxy)pentyloxy]-5,5,8,8-tetramethyl-5,6,7,8-tetrahydro-2-naphthaleneboronic acid (300 mg, 0.67 mmol), a 2M solution of potassium carbonate in water (0.67 ml) and methyl (Z)-3-iodo-2-butenoate (Ma, S. & Lu, X.; J. Chem. Soc. Chem. Com., pp. 1643-1644 (1990)) (182 mg) in dimethoxyethane (DME) (10 ml) was heated to reflux for 24 h. The solution was poured into a mixture of water and ethyl acetate. The organic phase was washed twice with water, dried over magnesium sulfate and concentrated in a rotary evaporator under vacuum at 40° C. The desired compound was purified by flash chromatography on a silica column.

WORKUP

后处理

  1. temperatureto reflux for 24 h
  2. washThe organic phase was washed twice with water
  3. dry with materialdried over magnesium sulfate
  4. concentrationconcentrated in a rotary evaporator under vacuum at 40° C
  5. customThe desired compound was purified by flash chromatography on a silica column