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Dimethylformamide → Sodium 2-[[[5-[[(2,5-dioxo-1-pyrolidinyl)oxy]carbonyl]-2-pyridinyl] hydrazono]methyl]-benzenesulfonate

HRID 2228528
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HRID 2228528 반응식
[Na+:1].[CH:2]([C:4]1[CH:9]=[CH:8][CH:7]=[CH:6][C:5]=1[S:10]([O-:13])(=[O:12])=[O:11])=O.N(C1N=CC=CC=1[C:18](O)=[O:19])N.[OH:25][N:26]1[C:30](=[O:31])[CH2:29][CH2:28][C:27]1=[O:32].C1([N:39]=[C:40]=[N:41][CH:42]2[CH2:47][CH2:46][CH2:45]CC2)CCCCC1.C[N:49](C)C=O>CO>[O:32]=[C:27]1[CH2:28][CH2:29][C:30](=[O:31])[N:26]1[O:25][C:18]([C:47]1[CH:46]=[CH:45][C:40]([NH:39][N:49]=[CH:2][C:4]2[CH:9]=[CH:8][CH:7]=[CH:6][C:5]=2[S:10]([O-:13])(=[O:12])=[O:11])=[N:41][CH:42]=1)=[O:19].[Na+:1]
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참가 물질

7

반응물 5

HCID 6228DimethylformamideHCID 10868DicyclohexylcarbodiimideHCID 80170N-HydroxysuccinimideHCID 585323Hydrazinonicotinic acidHCID 3794540Sodium o-formylbenzenesulfonate

생성물 1

HCID 59642097Sodium 2-[[[5-[[(2,5-dioxo-1-pyrolidinyl)oxy]carbonyl]-2-pyridinyl] hydrazono]methyl]-benzenesulfonate

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

To a solution of 2-formylbenzenesulfonic acid sodium salt (13.6 g) in dimethylformamide (400 mL) was added 2-hydrazinonicotinic acid (10.0 g) and the mixture stirred for three hours. N-hydroxysuccinimide (7.52 g) and dicyclohexylcarbodiimide (27.6 g) were added to the reaction and it was stirred for 16 hours. The mixture was filtered through Celite and the filtrate concentrated under vacuum to a thick oil. This was triturated with ethyl acetate to afford a solid which was filtered to afford crude product (32.8 g). The solids were refluxed in hot methanol for 5 hours, filtered, washed with methanol, and dried under vacuum to afford Sodium 2-[[[5-[[(2,5-dioxo-1-pyrolidinyl)oxy]carbonyl]-2-pyridinyl]hydrazono]methyl]-benzenesulfonate (21.2 g) as a pale yellow solid. NMR (DMSO-d6): 2.88, s (4H); 7.36, m (3H); 7.79, d of d (1H); 8.10, m (2H); 8.79, t (1H); 9.16, s (1H); 11.90, s (1H).

후처리

  1. stirringwas stirred for 16 hours
  2. filtrationThe mixture was filtered through Celite
  3. concentrationthe filtrate concentrated under vacuum to a thick oil
  4. customThis was triturated with ethyl acetate
  5. customto afford a solid which
  6. filtrationwas filtered
  7. customto afford crude product (32.8 g)
  8. filtrationfiltered
  9. washwashed with methanol
  10. customdried under vacuum

출처 및 근거

ORD 기록
ord-95bb91ba427947f6bec2e3f9a747523e
출처 데이터셋
uspto-grants-2002_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06416733B1

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