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Dimethylformamide → 3-(1-METHYL-5-NITRO-2-IMIDAZOLYL)-6-FORMYLAMINO-S-TRIAZOLO [4,3-b]PYRIDAZINE

HRID 1729864
ノート
印刷プレビュー

反応式

HRID 1729864 の反応式
[N+:1]([C:4]1[N:8]([CH3:9])[C:7]([C:10]2[N:14]3[N:15]=[C:16]([NH2:19])[CH:17]=[CH:18][C:13]3=[N:12][N:11]=2)=[N:6][CH:5]=1)([O-:3])=[O:2].CN(C)[CH:22]=[O:23].C(OC(=O)C)(=O)C>C(O)=O>[CH3:9][N:8]1[C:4]([N+:1]([O-:3])=[O:2])=[CH:5][N:6]=[C:7]1[C:10]1[N:14]2[N:15]=[C:16]([NH:19][CH:22]=[O:23])[CH:17]=[CH:18][C:13]2=[N:12][N:11]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 6228DimethylformamideHCID 7918Acetic AnhydrideHCID 214559243-(5-Nitro-1-methyl-2-imidazolyl)-6-amino-s-triazolo[4,3-b]pyridazine

生成物 1

HCID 214560043-(1-METHYL-5-NITRO-2-IMIDAZOLYL)-6-FORMYLAMINO-S-TRIAZOLO [4,3-b]PYRIDAZINE

試薬・触媒・溶媒 1

HCID 284Formic Acid溶媒

実験手順

100 mg. 3-(5-nitro-1-methyl-2-imidazolyl)-6-amino-s-triazolo [4,3-b]pyridazine were suspended in 1.3 ml. dimethyl formamide and, after the addition of 1.5 ml. of the mixed anhydride obtainable from formic acid and acetic anhydride, stirred at ambient temperature until no more starting material could be detected by thin layer chromatography. The almost clear solution thus obtained was, after filtration, evaporated in a vacuum and the residue brought to crystallization with ether. There were thus obtained 72 mg. (65 percent of theory) 3-(1-methyl-5-nitro-2-imidazolyl)-6-formylamino-s-triazolo[4,3-b]pyridazine in the form of yellowish crystals which melt, with decomposition, at 200° - 204° C.

後処理

  1. customThe almost clear solution thus obtained
  2. filtrationafter filtration
  3. customevaporated in a vacuum
  4. customthe residue brought to crystallization with ether
  5. customat 200° - 204° C.

出典と根拠

ORDレコード
ord-695898540b1347618a12eb1d229d7f9c
出典データセット
uspto-grants-1976_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US03989832

反応ノート

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