反応 #76504

ord-da20f6b9c3c44a1780128c8672b4caa0

反応方程式

CCN1CCc2c([N+](=O)[O-])cc3[nH]c(=O)c(=O)[nH]c3c2C1
product
CCN1CCc2c([N+](=O)[O-])cc3[nH]c(=O)c(=O)[nH]c3c2C1
9-Ethyl-1,4,7,8,9,10-hexahydro-6-nitro-pyrido[3,4-f]quinoxaline-2,3-dione
CS(=O)(=O)O
methanesulfonic acid
→
CCN1CCc2c([N+](=O)[O-])cc3[nH]c(=O)c(=O)[nH]c3c2C1.CS(=O)(=O)O
title compound
収率 92.0%
CCN1CCc2c([N+](=O)[O-])cc3[nH]c(=O)c(=O)[nH]c3c2C1.CS(=O)(=O)O
9-Ethyl-1,4,7,8,9,10-hexahydro-6-nitro-pyrido-[3,4-f]quinoxaline-2,3-dione methanesulfonate
収率 92.0%

反応物

CCN1CCc2c([N+](=O)[O-])cc3[nH]c(=O)c(=O)[nH]c3c2C1
product
CCN1CCc2c([N+](=O)[O-])cc3[nH]c(=O)c(=O)[nH]c3c2C1
9-Ethyl-1,4,7,8,9,10-hexahydro-6-nitro-pyrido[3,4-f]quinoxaline-2,3-dione
CS(=O)(=O)O
methanesulfonic acid

試薬

なし

溶媒

CN(C)C=O
dimethylformamide

反応条件

温度
100°CELSIUS
詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    workup.DISSOLUTIONdissolved
  2. 2
    その他Solvent was evaporated in vacuo
  3. 3
    洗浄the yellow residue washed with acetone
  4. 4
    乾燥dried under vacuum over P2O5

実験手順

The product from Example 74 was suspended in 300 mL dimethylformamide and 1 mL of 3 N methanesulfonic acid added. The suspension was warmed to 100° C. The colour changed from orange to yellow and all of the solid dissolved. Solvent was evaporated in vacuo, the yellow residue washed with acetone and then dried under vacuum over P2O5 to give the title compound (0.73 g, 92% yield) mp=302-304° C.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US06703391B2uspto-grants-2004_03