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Sodium Hydroxide → 5-Amino-3-(4-tolyl)-1-(3-trifluoromethoxyphenyl)pyrazole-4-carboxamide

HRID 582007
ノート
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反応式

HRID 582007 の反応式
[OH-].[Na+].Cl.[F:4][C:5]([F:16])([F:15])[O:6][C:7]1[CH:8]=[C:9]([NH:13][NH2:14])[CH:10]=[CH:11][CH:12]=1.[C:17]([C:19](=[C:23](SC)[C:24]1[CH:29]=[CH:28][C:27]([CH3:30])=[CH:26][CH:25]=1)[C:20]([NH2:22])=[O:21])#[N:18]>C(O)C>[NH2:18][C:17]1[N:13]([C:9]2[CH:10]=[CH:11][CH:12]=[C:7]([O:6][C:5]([F:15])([F:16])[F:4])[CH:8]=2)[N:14]=[C:23]([C:24]2[CH:29]=[CH:28][C:27]([CH3:30])=[CH:26][CH:25]=2)[C:19]=1[C:20]([NH2:22])=[O:21]
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 3

HCID 14798Sodium HydroxideHCID 45046393(3-(Trifluoromethoxy)phenyl)hydrazine hydrochlorideHCID 542422372-Cyano-3-methylthio-3-(4-tolyl)acrylamide

生成物 1

HCID 545661205-Amino-3-(4-tolyl)-1-(3-trifluoromethoxyphenyl)pyrazole-4-carboxamide収率 42.5%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

Powdered sodium hydroxide (88 mg, 2.2 mmol) was added to a solution of 3-trifluoromethoxyphenyl hydrazine hydrochloride (503 mg, 2.2 mmol) and 2-cyano-3-methylthio-3-(4-tolyl)acrylamide (464 mg, 2.0 mmol) in ethanol (20 ml) and the mixture heated at reflux for 18 h. On cooling, the solvent was removed under reduced pressure and the residue partitioned between water (80 ml) and ethyl acetate (100 ml). The aqueous layer was further extracted with ethyl acetate (2×80 ml) and the combined organic layers washed with brine (100 ml), dried (MgSO4) and concentrated under reduced pressure. The crude product was recrystallised from isopropyl ether-heptane to give the title compound as white needles (320 mg) m.p. 177-179°. δH (CDCl3) 7.70 (1H, m), 7.51 (1H, d, J 8.0 Hz), 7.38 (1H, d, J 8.0 Hz), 7.40 (1H, m), 7.09 (1H, d, J 7.9 Hz), 5.74 (2H, br s), 5.35 (2H, br s) and 2.42 (9H, s).

後処理

  1. temperaturethe mixture heated
  2. temperatureat reflux for 18 h
  3. temperatureOn cooling
  4. customthe solvent was removed under reduced pressure
  5. customthe residue partitioned between water (80 ml) and ethyl acetate (100 ml)
  6. extractionThe aqueous layer was further extracted with ethyl acetate (2×80 ml)
  7. washthe combined organic layers washed with brine (100 ml)
  8. dry with materialdried (MgSO4)
  9. concentrationconcentrated under reduced pressure
  10. customThe crude product was recrystallised from isopropyl ether-heptane

出典と根拠

ORDレコード
ord-f02fe20915ec4309a734091ec3fedc13
出典データセット
uspto-grants-1999_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05922741

反応ノート

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