HRID1264550

反应详情

EQUATION

反应方程式

HRID 1264550 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Combine 2-(4-amino-3-oxo-1,3,4,5-tetrahydro-benzo[c]azepin-2-yl)-4-methyl-valeric acid, tert-butyl ester (0.34 mmol), 2-bromo-6-phthalimidohexanoic acid (0.189 g, 0.56 mmol), 1-(3-dimethylaminopropyl)-3-ethylcarbodiimide hydrochloride (0.106 g, 0.55 mmol), and 1-hydroxybenztriazole hydrate ((75 mg, 0.56 mmol) in dicloromethane (8 mL). After 17 hours, evapoarte in vacuo to give a residue, partition the residue between ethyl aceate and an aqueous 5% sulfuric acid solution (about 20 mL). Separate the layers, extract the organic layer with a saturate aqueiosu sodium bicarbonate solution and then brine, dry over Na2SO4, filter, and evaporate in vacuo to give the title compound.

WORKUP

后处理

  1. customevapoarte in vacuo to give a residue
  2. custompartition the residue between ethyl aceate
  3. customSeparate the layers
  4. extractionextract the organic layer with a saturate aqueiosu sodium bicarbonate solution
  5. dry with materialbrine, dry over Na2SO4
  6. filtrationfilter
  7. customevaporate in vacuo