HRID1435587

反应详情

EQUATION

反应方程式

HRID 1435587 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
70 °C

PROCEDURE

实验过程

Potassium tert-butoxide (1.18 g, 10.5 mmol) was added to a solution of 3-[3-(2-methoxy-ethoxy)-phenylethynyl]-5-nitro-pyridin-2-ylamine (1.57 g, 5 mmol) in a 2:1 mixture of tetrahydrofuran and dimethylformamide (75 mL). The mixture was heated at 70° C. for 16 hours then the tetrahydrofuran was removed in vacuo. The mixture was poured onto a pad of silica and eluted with ethyl acetate then 10% methanol in ethyl acetate. The organics were concentrated in vacuo to 5% of their original volume and water (30 mL) was added. The resultant orange solid was filtered and dried to afford 2-[3-(2-methoxy-ethoxy)-phenyl]-5-nitro-1H-pyrrolo[2,3-b]pyridine (1.3 g, 83%).

WORKUP

后处理

  1. customthe tetrahydrofuran was removed in vacuo
  2. additionThe mixture was poured onto a pad of silica
  3. washeluted with ethyl acetate
  4. concentrationThe organics were concentrated in vacuo to 5% of their original volume and water (30 mL)
  5. additionwas added
  6. filtrationThe resultant orange solid was filtered
  7. customdried