Hydrochloric Acid → HCID 12888761, 화합물

HRID 1153848노트

반응식

HRID 1153848 반응식
[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

참가 물질

8

반응물 5

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

생성물 1

HCID 12888761HCID 12888761, 화합물

시약·촉매·용매 2

HCID 21218Trioctylmethylammonium chloride촉매HCID 1140Toluene용매

실험 절차

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.

후처리

  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)

출처 및 근거

ORD 기록
ord-3358a32e5f894ba1ad957872b767d9eb
출처 데이터셋
uspto-grants-1984_12
특허 번호
US04486591

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