HRID2079751

反应详情

EQUATION

反应方程式

HRID 2079751 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Heat a stirred mixture of 2,6-dibromopyridine (15; g, 63; mmol) and dimethylamine (40% aqueous solution, 21.4; mL, 190; mmol, 3; equiv) in ethanol (75; mL) for 3; days at 70° C. Evaporate the yellow solution to a reduced volume and dilute with ethyl acetate (100; mL). Wash with water (40; mL), brine (40; mL) and dry over sodium sulfate. Decant the liquid and evaporate to give pale yellow oil (13.8; g). Distill using a Kügelrohr apparatus to give the title product as a colorless liquid (12.4; g, b.p.=100-140° C. at 0.1 mbar). MS (m/z): 201, 203; (M+1).

WORKUP

后处理

  1. temperatureHeat
  2. customat 70° C
  3. customEvaporate the yellow solution to a reduced volume
  4. additiondilute with ethyl acetate (100; mL)
  5. washWash with water (40; mL), brine (40; mL)
  6. dry with materialdry over sodium sulfate
  7. customDecant the liquid
  8. customevaporate
  9. customto give pale yellow oil (13.8; g)
  10. distillationDistill