HRID1943779

反应详情

EQUATION

反应方程式

HRID 1943779 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of (1S)-1-pyridin-3-ylbutan-1-amine (600 mg, 4.0 mmol) in ethanol (20 mL) was added 2,4-dichloro-5-methylpyrimidine (717 mg, 4.4 mmol) and diisopropylethylamine (1.4 mL, 8 mmol). The solution was heated at reflux for 24 h after which time the solvent was removed under reduced pressure. The residue was dissolved in ethyl acetate (30 mL) and washed with H2O (2×15 mL), brine (15 mL) and dried (Na2SO4). The residue remaining after concentration in vacuo was chromatographed using ethyl acetate-hexanes (9:1) as eluant to separate the desired product (370 mg).

WORKUP

后处理

  1. temperatureThe solution was heated
  2. temperatureat reflux for 24 h after which time the solvent
  3. customwas removed under reduced pressure
  4. dissolutionThe residue was dissolved in ethyl acetate (30 mL)
  5. washwashed with H2O (2×15 mL), brine (15 mL)
  6. dry with materialdried (Na2SO4)
  7. concentrationafter concentration in vacuo
  8. customwas chromatographed
  9. customto separate the desired product (370 mg)