HRID1454808

反应详情

EQUATION

反应方程式

HRID 1454808 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

2-Amino-6-bromopyridine (2 g) was dissolved in dioxane (50 mL), and at 0° C. under an argon athmosphere 1,3-bis(diphenylphosphino)propane nickel (II) chloride (0.627 g) was added followed by diisopropyl zinc (23.12 mL of a 1M solution in toluene, via syringe over 30 minutes). The mixture was allowed to reflux for 15 h, poured into 2-propanol, which was then concentrated in vacuo. The residue was partitioned between AcOEt and saturated aqueous NH4Cl solution, the layers were separated and the organic layer dried over Na2SO4, filtered and evaporated. The residue was purified by flash chromatography (methylene chloride/methanol 95:5) to give 6-isopropyl-pyridin-2-ylamine as light brown oil (0.48 g). MS (EI): 136.1 (M+).

WORKUP

后处理

  1. additionat 0° C. under an argon athmosphere 1,3-bis(diphenylphosphino)propane nickel (II) chloride (0.627 g) was added
  2. temperatureto reflux for 15 h
  3. concentrationwas then concentrated in vacuo
  4. customThe residue was partitioned between AcOEt and saturated aqueous NH4Cl solution
  5. customthe layers were separated
  6. dry with materialthe organic layer dried over Na2SO4
  7. filtrationfiltered
  8. customevaporated
  9. customThe residue was purified by flash chromatography (methylene chloride/methanol 95:5)