HRID1662819

反应详情

EQUATION

反应方程式

HRID 1662819 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

5-Bromo-pyridine-2-carboxylic acid (0.81 g, 4 mmol) was combined with 2-chloro-4,6-dimethoxy-1,3,5-triazine (CDMT) (0.85 g, 4.8 mmol) and diluted with DCM (20 mL). This was immediately treated with 4-methyl morpholine (0.81 g, 8 mmol) and allowed to stir at ambient temperature for 1 h. 2-Pyrrolidin-1-yl-ethylamine (0.46 g, 4 mmol) was then added in one portion. Stirring was continued overnight. Reaction solvents were removed and residue was taken up in ethyl acetate and washed once with water. Aqueous phase was back extracted once with fresh ethyl acetate. Organic phases were combined, washed once with brine and dried over sodium sulfate. Filtration followed by rotary evaporation provided product as yellow oil which solidified upon standing. Yellowish solids (0.5 g, 42%)

WORKUP

后处理

  1. stirringStirring
  2. waitwas continued overnight
  3. customReaction solvents
  4. customwere removed
  5. washwashed once with water
  6. extractionAqueous phase was back extracted once with fresh ethyl acetate
  7. washwashed once with brine
  8. dry with materialdried over sodium sulfate
  9. filtrationFiltration
  10. customfollowed by rotary evaporation
  11. customprovided product as yellow oil which