Reaktion #44449

ord-0c8f183d36644254954c8daa0d4dd659

Reaktionsgleichung

COCCN[C@@H]1CCCN2c3c(ccc(Cl)c3Cl)Oc3ccccc3[C@H]12
trans-6,7-dichloro-2,3,4,14b-tetrahydro-N-(2-methoxyethyl)-1H-dibenzo[b,f]pyrido[1,2-d][1,4]oxazepine-1-amine
CCOC=O
ethyl formate
→
O=CN[C@@H]1CCCN2c3c(ccc(Cl)c3Cl)Oc3ccccc3[C@H]12
title compound
Ausbeute 30.0%
O=CN[C@@H]1CCCN2c3c(ccc(Cl)c3Cl)Oc3ccccc3[C@H]12
trans-N-(6,7-Dichloro-2,3,4,14b-tetrahydro-1H-dibenzo[b,f]pyrido[1,2-d][1,4]oxazepin-1-yl)formamide
Ausbeute 30.0%

Edukte

COCCN[C@@H]1CCCN2c3c(ccc(Cl)c3Cl)Oc3ccccc3[C@H]12
trans-6,7-dichloro-2,3,4,14b-tetrahydro-N-(2-methoxyethyl)-1H-dibenzo[b,f]pyrido[1,2-d][1,4]oxazepine-1-amine
CCOC=O
ethyl formate

Reagenzien

Keine

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Temperaturat reflux temperature
  2. 2
    SonstigeAfter removal of the solvent under reduced pressure
  3. 3
    Sonstigethe remaining product was purified with preparative LC-MS

Vorschrift

A solution of trans-6,7-dichloro-2,3,4,14b-tetrahydro-N-(2-methoxyethyl)-1H-dibenzo[b,f]pyrido[1,2-d][1,4]oxazepine-1-amine (122 mg, 0.36 mmol) in ethyl formate was stirred overnight at reflux temperature. After removal of the solvent under reduced pressure, the remaining product was purified with preparative LC-MS to give the title compound (40 mg, 30%). Data (m/z)=397 (M+H)+.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US07737136B2uspto-grants-2010_06