تفاعل #44449

ord-0c8f183d36644254954c8daa0d4dd659

معادلة التفاعل

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
المردود 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
المردود 30.0%

المتفاعلات

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

الكواشف

لا شيء

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    درجة الحرارةat reflux temperature
  2. 2
    أخرىAfter removal of the solvent under reduced pressure
  3. 3
    أخرىthe remaining product was purified with preparative LC-MS

الإجراء التجريبي

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)+.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US07737136B2uspto-grants-2010_06