Methanesulfonic Acid → 9-Ethyl-1,4,7,8,9,10-hexahydro-6-nitro-pyrido-[3,4-f]quinoxaline-2,3-dione Methanesulfonate

HRID 48226ノート

反応式

HRID 48226 の反応式
[CH2:1]([N:3]1[CH2:16][CH2:15][C:14]2[C:13]([N+:17]([O-:19])=[O:18])=[CH:12][C:11]3[NH:10][C:9](=[O:20])[C:8](=[O:21])[NH:7][C:6]=3[C:5]=2[CH2:4]1)[CH3:2].[CH3:22][S:23]([OH:26])(=[O:25])=[O:24]>CN(C)C=O>[CH3:22][S:23]([OH:26])(=[O:25])=[O:24].[CH2:1]([N:3]1[CH2:16][CH2:15][C:14]2[C:13]([N+:17]([O-:19])=[O:18])=[CH:12][C:11]3[NH:10][C:9](=[O:20])[C:8](=[O:21])[NH:7][C:6]=3[C:5]=2[CH2:4]1)[CH3:2]

参加物

4

反応物 2

HCID 6395Methanesulfonic AcidHCID 10266209(9S)-9-ethyl-3-hydroxy-6-nitro-7,8,9,10-tetrahydropyrido[3,4-f]quinoxalin-9-ium-2-olate

生成物 1

HCID 227424649-Ethyl-1,4,7,8,9,10-hexahydro-6-nitro-pyrido-[3,4-f]quinoxaline-2,3-dione Methanesulfonate収率 92%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

反応条件

温度
100 °C

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.

後処理

  1. dissolutiondissolved
  2. customSolvent was evaporated in vacuo
  3. washthe yellow residue washed with acetone
  4. dry with materialdried under vacuum over P2O5

出典と根拠

ORDレコード
ord-da20f6b9c3c44a1780128c8672b4caa0
出典データセット
uspto-grants-2004_03
特許番号
US06703391B2

反応ノート

読み込み中…