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Hydrazine hydrate (1:1) → 2-(5-Amino-3-methyl-1H-pyrazol-4-yl)benzothiazole-5-sulfonic acid methylamide

HRID 2261640
ノート
印刷プレビュー

反応式

HRID 2261640 の反応式
[CH3:1][NH:2][S:3]([C:6]1[CH:7]=[CH:8][C:9]2[S:13][C:12]([C:14]([C:19]#[N:20])=[C:15](OC)[CH3:16])=[N:11][C:10]=2[CH:21]=1)(=O)=[O:4].[OH2:22].[NH2:23][NH2:24]>CO.Cl>[CH3:1][NH:2][S:3]([C:6]1[CH:7]=[CH:8][C:9]2[S:13][C:12]([C:14]3[C:15]([CH3:16])=[N:23][NH:24][C:19]=3[NH2:20])=[N:11][C:10]=2[CH:21]=1)(=[O:4])=[O:22]
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 2

HCID 24654Hydrazine hydrate (1:1)HCID 667682252-(1-Cyano-2-methoxypropenyl)benzothiazole-5-sulfonic acid methylamide

生成物 1

HCID 1784862662-(5-Amino-3-methyl-1H-pyrazol-4-yl)benzothiazole-5-sulfonic acid methylamide収率 43%

試薬・触媒・溶媒 2

HCID 313Hydrochloric Acid触媒HCID 887Methanol溶媒

実験手順

To a suspension of 2-(1-cyano-2-methoxypropenyl)benzothiazole-5-sulfonic acid methylamide (120 mg, 0.37 mmol) in 4 mL of methanol, was added hydrazine hydrate (20 μL). The mixture was heated to reflux for 5 hrs and then 1 drop of conc. hydrochloric acid was added to the reaction mixture. The mixture was refluxed for an additional 5 min and was then allowed to cool. The volume of solvent was reduced under reduced pressure and a solid formed. The solid was isolated by filtration and was washed with methanol and then water and dried to yield 51 mg (43%) of the title compound as a cream coloured powder. MS (m/z, ES+): 324.0 (M+1, 100%).

後処理

  1. temperatureThe mixture was heated
  2. temperatureto reflux for 5 hrs
  3. temperatureThe mixture was refluxed for an additional 5 min
  4. temperatureto cool
  5. customa solid formed
  6. customThe solid was isolated by filtration
  7. washwas washed with methanol
  8. dry with materialwater and dried

出典と根拠

ORDレコード
ord-6d2fcaaa185c4765ae44375d18f56ac1
出典データセット
uspto-grants-2010_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07847101B2

反応ノート

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