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

HRID 2228528
ノート
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反応式

HRID 2228528 の反応式
[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]
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 5

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-95bb91ba427947f6bec2e3f9a747523e
出典データセット
uspto-grants-2002_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06416733B1

反応ノート

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