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

HRID 476555노트

반응식

HRID 476555 반응식
[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

참가 물질

5

반응물 3

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

생성물 1

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

시약·촉매·용매 1

HCID 702Ethanol용매2회

실험 절차

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%).

후처리

  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

출처 및 근거

ORD 기록
ord-a4b5bc3cb66740678b49da862962aa8b
출처 데이터셋
uspto-grants-1989_12
특허 번호
US04885272

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