反应 #1269899

ord-10ba122504654e85b39d5e3e53cffcf4

反应方程式

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
收率 84.0%
Clc1ccc2c(c1)CNCc1nnc(Br)n1-2
1-Bromo-8-chloro-5,6-dihydro-4H-2,3,5,10b-tetraaza-benzo[e]azulene
收率 84.0%

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    萃取extracted with ethyl acetate
  2. 2
    洗涤The organic layer was washed with brine
  3. 3
    干燥dried over anhydrous sodium sulfate
  4. 4
    浓缩concentrated in vacuo

实验过程

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+).

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US08664216B2uspto-grants-2014_03