HRID852860

反应详情

EQUATION

反应方程式

HRID 852860 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A suspension of lithium aluminum hydride (263 mg, 6.92 mmol) in THF (20 mL) was added slowly to [1-(methoxy-methyl-carbamoyl)-2-(1-trityl-1H-imidazol-4-yl)-ethyl]-carbamic acid tert-butyl ester (3.4 g, 6.3 mmol) in THF (75 mL) at −20° C. The reaction was complete (silica gel, EA, Rf 0.48) in 15 minutes. Saturated sodium potassium tartrate (10 mL) was added, and the solvent removed. Water was added and the residue extracted with Et2O. The Et2O was washed with brine, dried and filtered. Removal of the solvent gave the title compound (2.552 g, 84%). ESMS 482 (M+H+) 1H NMR ( ) 13C NMR ( )

WORKUP

后处理

  1. customin 15 minutes
  2. customthe solvent removed
  3. additionWater was added
  4. extractionthe residue extracted with Et2O
  5. washThe Et2O was washed with brine
  6. customdried
  7. filtrationfiltered
  8. customRemoval of the solvent