Acetic Acid → 3-tert-butyl-1-phenyl-1H-pyrazol-5-amine

HRID 476555

反応式

HRID 476555 の反応式
[C:1]([CH2:7][C:8]#[N:9])(=O)[C:2]([CH3:5])([CH3:4])[CH3:3].[C:10]1([NH:16][NH2:17])[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=1.C(O)(=O)C>C(O)C>[NH2:9][C:8]1[N:16]([C:10]2[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=2)[N:17]=[C:1]([C:2]([CH3:5])([CH3:4])[CH3:3])[CH:7]=1

参加物

5

反応物 3

HCID 176Acetic AcidHCID 7516PhenylhydrazineHCID 108871Pentanenitrile, 4,4-dimethyl-3-oxo-

生成物 1

HCID 7706343-tert-butyl-1-phenyl-1H-pyrazol-5-amine

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒2 回

実験手順

Pivaloyl acetonitrile (30.0 g; 0.24 mole) and ethanol (200 ml) were placed into a 500 ml round bottom flask. Phenylhydrazine (23.6 ml; 0.24 mole) was added with stirring followed by acetic acid (13.8 ml). The reaction was refluxed for 5 hours. Part of the ethanol was stripped off and the residue was poured into ice water. The product was filtered off and washed with water. The solid was dissolved in hot ethanol (100 ml), diluted with water, stirred, filtered, and washed with water. The yield of solid, m.p. 65°-7° C. was 46.3 g (90%).

後処理

  1. temperatureThe reaction was refluxed for 5 hours
  2. filtrationThe product was filtered off
  3. washwashed with water
  4. dissolutionThe solid was dissolved in hot ethanol (100 ml)
  5. additiondiluted with water
  6. stirringstirred
  7. filtrationfiltered
  8. washwashed with water

出典と根拠

ORDレコード
ord-a4b5bc3cb66740678b49da862962aa8b
出典データセット
uspto-grants-1989_12
特許番号
US04885272

関連ノート

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