HRID2369460

反应详情

EQUATION

反应方程式

HRID 2369460 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

Methyl 3,5-diaminobenzoate (260.8 mg, 1.9 mmol) is dissolved in dry tetrahydrofuran (5 mL) in a 100 mL vessel under an inert atmosphere. Triethylamine (0.7 mL, 4.99 mmol) is then added and the solution is cooled to 0° C. A solution of 2-decyltetradecanoyl chloride from Step I in dry tetrahydrofuran (10 mL) is then added slowly, dropwise. The reaction is then allowed to slowly warm to room temperature. After stirring overnight, the reaction is quenched with water and the tetrahydrofuran is removed by rotary evaporation. The crude product residue is then dissolved in diethyl ether (50 mL) and is washed with deionized water (20 mL). The ether layer is separated and concentrated to give methyl 3,5-bis(2′-decyltetradecanamido)benzoate as a pale pink solid (1.17 g).

WORKUP

后处理

  1. temperatureto slowly warm to room temperature
  2. customthe reaction is quenched with water
  3. customthe tetrahydrofuran is removed by rotary evaporation
  4. dissolutionThe crude product residue is then dissolved in diethyl ether (50 mL)
  5. washis washed with deionized water (20 mL)
  6. customThe ether layer is separated
  7. concentrationconcentrated