HRID1247836

反应详情

EQUATION

反应方程式

HRID 1247836 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To a suspension of 3-{[1-methyl-5-(tritylamino)-1H-pyrazol-4-yl]amino}-3-oxopropanoic acid (600 mg) and tert-butyl (2-aminoethyl)carbamate (240 mg) in tetrahydrofuran (12 ml) and dichloromethane (6 ml) was added WSCD HCl (522 mg), and the whole mixture was stirred at room temperature overnight. To the reaction mixture was added water (3 ml), and the whole mixture was extracted with ethyl acetate. The extract was washed with water and brine and dried over magnesium sulfate. The evaporation of the solvent gave a crude residue, which was triturated with diisopropyl ether-ethyl acetate (2:1) to give tert-butyl {2-[(3-{[1-methyl-5-(tritylamino)-1H-pyrazol-4-yl]amino}-3-oxopropanoyl)amino]ethyl}carbamate (537 mg).

WORKUP

后处理

  1. extractionthe whole mixture was extracted with ethyl acetate
  2. washThe extract was washed with water and brine
  3. dry with materialdried over magnesium sulfate
  4. customThe evaporation of the solvent
  5. customgave a crude residue, which
  6. customwas triturated with diisopropyl ether-ethyl acetate (2:1)