HRID925467

反应详情

EQUATION

反应方程式

HRID 925467 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

5-Bromo-3-methyl-pyridine-2-carboxylic acid 1-dimethylamino-meth-(E)-ylideneamine (2.5 g, 9.25 mmol) was dissolved in THF (20 ml). KOtBu (1.565 g, 13.05 mmol) in THF (30 ml) was added dropwise and the reaction mixture was heated to reflux for 3 h and then cooled to rt. The pH was adjusted to 7 with concentrated HCl. The reaction mixture was concentrated. The brown solid obtained was triturated with water (10 ml). The solid thus obtained was collected by filtration (2 g, 8 mmol).

WORKUP

后处理

  1. temperaturethe reaction mixture was heated
  2. temperatureto reflux for 3 h
  3. concentrationThe reaction mixture was concentrated
  4. customThe brown solid obtained
  5. customwas triturated with water (10 ml)
  6. customThe solid thus obtained
  7. filtrationwas collected by filtration (2 g, 8 mmol)