HRID41799

反应详情

EQUATION

反应方程式

HRID 41799 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of methyl 2-(N-tert-butoxycarbonyl-N-{(2′-[1-benzyl-1H-tetrazol-5-yl]biphenyl-4-yl)methyl}amino)-3-nitrobenzoate (compound 20b, 11.93 g, 19.2 mmol) in methanol (15 mL) was added 2NHCl-MeOH (30 mL) under ice-cooling, and the mixture was stirred at the same temperature for 2 hr, and then overnight at room temperature. The reaction mixture was concentrated under reduced pressure, and to the residue were added methanol and diisopropyl ether. The resulting crystals were collected by filtration, washed with diisopropyl ether and hexane, and dried under reduced pressure to give methyl 2-[({2′-[1-benzyl-1H-tetrazol-5-yl]biphenyl-4-yl}methyl)amino]-3-nitrobenzoate (compound 21b) (8.64 g, 86%) as yellow crystals.

WORKUP

后处理

  1. temperaturecooling
  2. customovernight
  3. customat room temperature
  4. concentrationThe reaction mixture was concentrated under reduced pressure
  5. additionto the residue were added methanol and diisopropyl ether
  6. filtrationThe resulting crystals were collected by filtration
  7. washwashed with diisopropyl ether and hexane
  8. customdried under reduced pressure