HRID2073393

反应详情

EQUATION

反应方程式

HRID 2073393 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A mixture of 1,1-dimethyl-7-nitro-8-(1H-1,2,4-triazol-1-ylmethyl)-2(1H)-naphtho[2,1-b]furanone (0.035 g), glacial acetic acid (2 ml) and 10% palladium-on-carbon (0.01 g) was stirred under an atmosphere of hydrogen at room temperature and atmospheric pressure for 2 h. The mixture was filtered, the filtrate was evaporated to dryness under reduced pressure, and the residue was partitioned between ethyl acetate and equeous sodium hydrogen carbonate solution. The ethyl acetate phase was dried and evaporated to dryness under reduced pressure, and the residue was purified by flash chromatography using methanol:ethyl acetate, 1:99 v/v. as eluant, to give 7-amino-1,1-dimethyl-8-(1H-1,2,4-triazol-1-ylmethyl)-2(1H)-naphtho[2,1-b]furanone, m.p. 160°-163°.

WORKUP

后处理

  1. filtrationThe mixture was filtered
  2. customthe filtrate was evaporated to dryness under reduced pressure
  3. customthe residue was partitioned between ethyl acetate and equeous sodium hydrogen carbonate solution
  4. dry with materialThe ethyl acetate phase was dried
  5. customevaporated to dryness under reduced pressure
  6. customthe residue was purified by flash chromatography