HRID1365126

反应详情

EQUATION

反应方程式

HRID 1365126 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Tert-butyl 2-(methoxycarbonyl)furan-3-ylcarbamate 33 (1.14 g, 1.0 eq) was dissolved in dichloromethane (8 ml) and treated with trifluoroacetic acid (5 ml). Reaction mixture was stirred at room temperature for 3 h, and was then concentrated. Residue was dissolved in dichloromethane and washed with saturated aq. NaHCO3. The organic layer was dried (Na2SO4) and concentrated Mixture was extracted with ethyl acetate. The combined organic extracts were dried with Na2SO4 and concentrated. The crude reaction mixture was purified by flash chromatography to yield methyl 3-aminofuran-2-carboxylate 34 (574 mg, 86%): MS (Q1) 142 (M)+.

WORKUP

后处理

  1. customReaction mixture
  2. concentrationwas then concentrated
  3. dissolutionResidue was dissolved in dichloromethane
  4. washwashed with saturated aq. NaHCO3
  5. dry with materialThe organic layer was dried (Na2SO4)
  6. concentrationconcentrated Mixture
  7. extractionwas extracted with ethyl acetate
  8. dry with materialThe combined organic extracts were dried with Na2SO4
  9. concentrationconcentrated
  10. customThe crude reaction mixture
  11. customwas purified by flash chromatography