HRID1910146

反应详情

EQUATION

反应方程式

HRID 1910146 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A mixture of 4-(4-methoxycarbonylmethyl-1H-imidazol-2-ylazo)-benzoic acid methyl ester (2 mmol, 604 mg) synthesized above, platinum (IV) oxide (60 mg) and methanol (50 mL) was hydrogenated (60 psi) for two days (another portion of PtO2 was added after one day). Trifluoroacetic acid (TFA) (2 mmol, 0.15 mL) was added to the reaction mixture and it was filtered. The filtrate was concentrated and diluted with water, washed with ether (2×50 mL). Evaporation of the water from the aqueous solution gave the (2-Amino-1H-imidazol-4-yl)-acetic acid methyl ester as a TFA salt. (273.8 mg, 51%). LCMS: 156 (M+1)+.

WORKUP

后处理

  1. customfor two days
  2. additionwas added after one day)
  3. filtrationwas filtered
  4. concentrationThe filtrate was concentrated
  5. additiondiluted with water
  6. washwashed with ether (2×50 mL)
  7. customEvaporation of the water from the aqueous solution