تفاعل #1888

ord-1fc2f1e399f34cafb24dd477e3e8aa29

معادلة التفاعل

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
المردود 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
المردود 75.2%

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    workup.ADDITIONwere added
  2. 2
    استخلاصthe solution was extracted with ethyl acetate
  3. 3
    غسيلby washing with water
  4. 4
    أخرىafter which the solvent was removed
  5. 5
    أخرىthe residue was recrystallized

الإجراء التجريبي

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.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US05726306uspto-grants-1998_03