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

HRID 48226노트

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HRID 48226 반응식
[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]

참가 물질

4

반응물 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

생성물 1

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

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

반응 조건

온도
100 °C

실험 절차

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.

후처리

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

출처 및 근거

ORD 기록
ord-da20f6b9c3c44a1780128c8672b4caa0
출처 데이터셋
uspto-grants-2004_03
특허 번호
US06703391B2

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