Hydrochloric Acid → HCID 12888761、化合物

HRID 1995277ノート

反応式

HRID 1995277 の反応式
[NH2:1][C:2]1[C:6]([C:7]#[N:8])=[CH:5][N:4]([CH3:9])[N:3]=1.F[C:11]1[CH:16]=[CH:15][CH:14]=[CH:13][C:12]=1[N+:17]([O-:19])=[O:18].C(=O)([O-])[O-].[K+].[K+].[OH-].[Na+].Cl>C1(C)C=CC=CC=1.CCCCCCCC[N+](CCCCCCCC)(CCCCCCCC)C.[Cl-]>[CH3:9][N:4]1[CH:5]=[C:6]([C:7]#[N:8])[C:2]([NH:1][C:11]2[CH:16]=[CH:15][CH:14]=[CH:13][C:12]=2[N+:17]([O-:19])=[O:18])=[N:3]1

参加物

8

反応物 5

HCID 313Hydrochloric AcidHCID 11430Potassium CarbonateHCID 14798Sodium HydroxideHCID 738951-Fluoro-2-nitrobenzeneHCID 106542131-Methyl-3-amino-4-cyanopyrazole

生成物 1

HCID 12888761HCID 12888761、化合物

試薬・触媒・溶媒 2

HCID 21218Trioctylmethylammonium chloride触媒HCID 1140Toluene溶媒

実験手順

3-Amino-1-methylpyrazole-4-carbonitrile (Helv. Chim. Acta (1959) 42, 763) (7.5 g) and 2-fluoronitrobenzene (8.4 g) were stirred in toluene (120 ml) with Adogen 464 (3.0 g) and potassium carbonate (16.5 g) at 60° C. 50% Sodium hydroxide solution (0.1 ml) was added and the mixture was heated under reflux for 2 hours. The mixture was poured on to dilute hydrochloric acid, extracted, the aqueous layer washed with toluene and the combined extracts washed twice with water. After evaporation the residue was crystallised from ethanol (750 ml) to give the title compound, m.p. 172° C.

後処理

  1. temperaturethe mixture was heated
  2. temperatureunder reflux for 2 hours
  3. extractionextracted
  4. washthe aqueous layer washed with toluene
  5. washthe combined extracts washed twice with water
  6. customAfter evaporation the residue
  7. customwas crystallised from ethanol (750 ml)

出典と根拠

ORDレコード
ord-da45cec5632a4c7f8e8ab12dafd9e02e
出典データセット
uspto-grants-1983_09
特許番号
US04404137

反応ノート

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