HRID1187433

反应详情

EQUATION

反应方程式

HRID 1187433 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 2-bromo-1-(6-bromopyridin-3-yl)ethanone from Step A (2.3 g, 8.25 mmol) and pyridine-2-carboxamide (1 g, 8.25 mmol) was melted at 85°. Heating was continued until the mixture reached 140° at which point the product solidified. Ice, EtOAc and sat aq NaHCO3 were added. The aqueous layer was then back extracted with EtOAc/THF (3:1). Pooled organics were dried over MgSO4, filtered, concentrated, and purified on silica gel to afford 250 mg (10% yield) of 2-bromo-5-(2-pyridin-2-yl-1,3-oxazole-4-yl)pyridine. LC/MS: m/e 302.0 (M+H).

WORKUP

后处理

  1. temperatureHeating
  2. customreached 140° at which point
  3. additionwere added
  4. extractionThe aqueous layer was then back extracted with EtOAc/THF (3:1)
  5. dry with materialPooled organics were dried over MgSO4
  6. filtrationfiltered
  7. concentrationconcentrated
  8. custompurified on silica gel