HRID2364661

反应详情

EQUATION

反应方程式

HRID 2364661 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

Methyl 7-nitrobenzofuran-4-carboxylate 1f (820 mg, 3.70 mmol) was dissolved in 150 mL of methanol in an ice-water bath, added with (164 mg, 10%) palladium/carbon, methanol (0.3 mL). The resulting solution was subjected to hydrogenation for 16 hours at 3 atmosphere at room temperature. The resulting mixture was filtered and washed with 50 mL of methanol, concentrated under reduced pressure. The crude residue was recrystallised by the mixture solvent of 25 mL ethyl acetate and n-hexane (V/V=1:4) to obtain the title compound methyl 7-amino-2,3-dihydrobenzofuran-4-carboxylate 1g (446 mg, yield: 62.0%) as a gray solid.

WORKUP

后处理

  1. filtrationThe resulting mixture was filtered
  2. washwashed with 50 mL of methanol
  3. concentrationconcentrated under reduced pressure
  4. customThe crude residue was recrystallised by the mixture solvent of 25 mL ethyl acetate and n-hexane (V/V=1:4)