반응 #1888

ord-1fc2f1e399f34cafb24dd477e3e8aa29

반응 방정식

CC(C)CN1C(=O)[C@@H](CC(=O)O)O[C@H](c2ccccc2Cl)c2cc(Cl)ccc21
trans-7-chloro-5-(2-chlorophenyl)-1-isobutyl-2-oxo-1,2,3,5-tetrahydro-4,1-benzoxazepine-3-acetic acid
[Cl-].[NH4+]
ammonium chloride
CCN=C=NCCCN(C)C.Cl
1-ethyl-3-(3-dimethylaminopropyl)carbodiimide hydrochloride
CCN(CC)CC
triethylamine
CC(C)CN1C(=O)[C@@H](CC(N)=O)O[C@H](c2ccccc2Cl)c2cc(Cl)ccc21
crystal
수율 75.2%
CC(C)CN1C(=O)[C@@H](CC(N)=O)O[C@H](c2ccccc2Cl)c2cc(Cl)ccc21
Trans-7-chloro-5-(2-chlorophenyl)-1-isobutyl-2-oxo-1,2,3,5-tetrahydro-4,1-benzoxazepine-3-acetamide
수율 75.2%

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    workup.ADDITIONwere added
  2. 2
    추출the solution was extracted with ethyl acetate
  3. 3
    세척by washing with water
  4. 4
    기타after which the solvent was removed
  5. 5
    기타the residue was recrystallized

실험 절차

1.0 g of trans-7-chloro-5-(2-chlorophenyl)-1-isobutyl-2-oxo-1,2,3,5-tetrahydro-4,1-benzoxazepine-3-acetic acid and 0.5 g of ammonium chloride were dissolved in 8 mi of dimethylformamide, and 0.46 g of 1-ethyl-3-(3-dimethylaminopropyl)carbodiimide hydrochloride and 0.7 ml of triethylamine were added, followed by stirring at room temperature for 30 minutes. After water was added, the solution was extracted with ethyl acetate, followed by washing with water, after which the solvent was removed and the residue was recrystallized to yield 0.75 g of a crystal.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US05726306uspto-grants-1998_03