Hydrazine hydrate (1:1) → HCID 178432134、化合物

HRID 869676ノート

反応式

HRID 869676 の反応式
[CH3:1][C:2]1[C:3]([C:12](=O)[CH2:13][C:14]#[N:15])=[N:4][C:5]2[C:10]([N:11]=1)=[CH:9][CH:8]=[CH:7][CH:6]=2.O.[NH2:18][NH2:19].C(=O)(O)[O-].[Na+]>C(O)(=O)C.C(O)C.O>[CH3:1][C:2]1[C:3]([C:12]2[CH:13]=[C:14]([NH2:15])[NH:19][N:18]=2)=[N:4][C:5]2[C:10]([N:11]=1)=[CH:9][CH:8]=[CH:7][CH:6]=2

参加物

7

反応物 3

HCID 24654Hydrazine hydrate (1:1)HCID 516892Sodium BicarbonateHCID 67397893HCID 67397893、化合物

生成物 1

HCID 178432134HCID 178432134、化合物

試薬・触媒・溶媒 3

HCID 176Acetic Acid溶媒HCID 702Ethanol溶媒HCID 962Water溶媒

実験手順

A suspension of 3-(3-methylquinoxalin-2-yl)-3-oxopropanenitrile (45.8 g, 217 mmol) and hydrazine monohydrate (15.8 mL, 325 mmol) in acetic acid (109 mL) and ethanol (1083 mL) was refluxed for 17 h. After being cooled to ambient temperature, the reaction mixture was diluted with water (360 mL) and basified to pH 8 with sodium bicarbonate. The resulting precipitate was collected and washed with diisopropyl ether. The crude was diluted with methanol (1077 mL) and potassium carbonate (29.9 g), and then heated at 60° C. for 2 h. The precipitate was collected and washed with diisopropyl ether to give 3-(3-methylquinoxalin-2-yl)-1H-pyrazol-5-amine. MS (APCI): m/z 226 (M+H).

後処理

  1. temperaturewas refluxed for 17 h
  2. customThe resulting precipitate was collected
  3. washwashed with diisopropyl ether
  4. additionThe crude was diluted with methanol (1077 mL) and potassium carbonate (29.9 g)
  5. temperatureheated at 60° C. for 2 h
  6. customThe precipitate was collected
  7. washwashed with diisopropyl ether

出典と根拠

ORDレコード
ord-3df8457ac8c84cd3ab0e48f7ef693f10
出典データセット
uspto-grants-2015_03
特許番号
US08969376B2

反応ノート

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