Hydrazine hydrate (1:1) → N-[2-(5-amino-4-benzothiazol-2-yl-1H-pyrazol-3-ylamino)ethyl]acetamide

HRID 407304

反応式

HRID 407304 の反応式
[S:1]1[C:5]2[CH:6]=[CH:7][CH:8]=[CH:9][C:4]=2[N:3]=[C:2]1[C:10](=[C:13](SC)SC)[C:11]#[N:12].[C:18]([NH:21][CH2:22][CH2:23][NH2:24])(=[O:20])[CH3:19].O.[NH2:26][NH2:27]>C(O)C>[NH2:12][C:11]1[NH:27][N:26]=[C:13]([NH:24][CH2:23][CH2:22][NH:21][C:18](=[O:20])[CH3:19])[C:10]=1[C:2]1[S:1][C:5]2[CH:6]=[CH:7][CH:8]=[CH:9][C:4]=2[N:3]=1

参加物

5

反応物 3

HCID 24654Hydrazine hydrate (1:1)HCID 66082N-(2-aminoethyl)acetamideHCID 28077272-Benzothiazol-2-yl-3,3-bis-methylsulfanylacrylonitrile

生成物 1

HCID 66768089N-[2-(5-amino-4-benzothiazol-2-yl-1H-pyrazol-3-ylamino)ethyl]acetamide収率 66%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

A mixture of 2-benzothiazol-2-yl-3,3-bis-methylsulfanylacrylonitrile (200 mg, 0.74 mmol) and N-acetylethylenediamine (83 mg, 0.81 mmol) in ethanol (10 mL) was refluxed for 90 min. To this solution was added hydrazine hydrate (61 mg, 1.2 mmol), and the resulting mixture was refluxed overnight. Solids formed upon cooling. The resulting crystals were filtered and washed with ethanol to yield 150 mg (66%) of N-[2-(5-amino-4-benzothiazol-2-yl-1H-pyrazol-3-ylamino)ethyl]acetamide. MS (ES+): 317.1 (M+1, 100%).

後処理

  1. temperaturewas refluxed for 90 min
  2. temperaturethe resulting mixture was refluxed overnight
  3. customSolids formed
  4. temperatureupon cooling
  5. filtrationThe resulting crystals were filtered
  6. washwashed with ethanol

出典と根拠

ORDレコード
ord-b5d4131a4344486a8567c2aee6bb6873
出典データセット
uspto-grants-2014_06
特許番号
US08754233B2

関連ノート

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