تفاعل #1269899

ord-10ba122504654e85b39d5e3e53cffcf4

معادلة التفاعل

CC(C)(C)OC(=O)N1Cc2cc(Cl)ccc2-n2c(Br)nnc2C1
1-bromo-8-chloro-4H,6H-2,3,5,10b-tetraaza-benzoazulene-5-carboxylic acid tert-butyl ester
Cl
hydrogen chloride
Clc1ccc2c(c1)CNCc1nnc(Br)n1-2
title compound
المردود 84.0%
Clc1ccc2c(c1)CNCc1nnc(Br)n1-2
1-Bromo-8-chloro-5,6-dihydro-4H-2,3,5,10b-tetraaza-benzo[e]azulene
المردود 84.0%

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    استخلاصextracted with ethyl acetate
  2. 2
    غسيلThe organic layer was washed with brine
  3. 3
    تجفيفdried over anhydrous sodium sulfate
  4. 4
    تركيزconcentrated in vacuo

الإجراء التجريبي

A solution of 1-bromo-8-chloro-4H,6H-2,3,5,10b-tetraaza-benzoazulene-5-carboxylic acid tert-butyl ester (3.0 g, 7.6 mmol) in 1.25 M methanolic hydrogen chloride solution (60 ml, 76 mmol) was heated at 50° C. for 10 min. The reaction mixture was poured on 1 M aqueous sodium hydroxide solution (200 ml) and extracted with ethyl acetate. The organic layer was washed with brine, dried over anhydrous sodium sulfate and concentrated in vacuo to give the title compound (1.9 g, 84%) as light yellow solid. MS m/e: 255 (M+H+).

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US08664216B2uspto-grants-2014_03