Water → HCID 178443176, Verbindung

HRID 444592Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 444592
[Cl:1][C:2]1[CH:7]=[C:6]([Cl:8])[CH:5]=[C:4]([Cl:9])[C:3]=1[N:10]1[C:14](=[O:15])[CH2:13][C:12]([NH:16][C:17]2[CH:22]=[C:21]([NH:23][C:24](=[O:38])[CH2:25][CH2:26][CH2:27][CH2:28][CH2:29][CH2:30][CH2:31][CH2:32][CH2:33][CH2:34][CH2:35][CH2:36][CH3:37])[CH:20]=[CH:19][C:18]=2[Cl:39])=[N:11]1.C(=O)([O-])[O-].[K+].[K+].Cl.[CH2:47]([S:54]SC(=N)N)[C:48]1[CH:53]=[CH:52][CH:51]=[CH:50][CH:49]=1.O>C(O)C>[Cl:9][C:4]1[CH:5]=[C:6]([Cl:8])[CH:7]=[C:2]([Cl:1])[C:3]=1[N:10]1[C:14](=[O:15])[CH:13]([S:54][CH2:47][C:48]2[CH:53]=[CH:52][CH:51]=[CH:50][CH:49]=2)[C:12]([NH:16][C:17]2[CH:22]=[C:21]([NH:23][C:24](=[O:38])[CH2:25][CH2:26][CH2:27][CH2:28][CH2:29][CH2:30][CH2:31][CH2:32][CH2:33][CH2:34][CH2:35][CH2:36][CH3:37])[CH:20]=[CH:19][C:18]=2[Cl:39])=[N:11]1

Komponenten

6

Edukt 4

HCID 962WaterHCID 11430Potassium CarbonateHCID 23464086S-benzylthioisothiourea hydrochlorideHCID 178443172N-[4-chloro-3-[[5-oxo-1-(2,4,6-trichlorophenyl)-4H-pyrazol-3-yl]amino]phenyl]tetradecanamide

Produkt 1

HCID 178443176HCID 178443176, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 702EthanolLösungsmittel

Versuchsvorschrift

1-(2,4,6-trichlorophenyl)-3-(2-chloro-5-tetradecanamidoanilino)-5-oxo-2-pyrazoline (21.4 g) was dissolved in 80% ethanol (ratio by volume of water:20%), and 2.42 g of anhydrous potassium carbonate was added thereto. The solution was refluxed with heating. 8.2 g of S-benzylthioisothiourea hydrochloride was added to the solution and the solution was vigorously stirred for 3 hours. After confirming the conclusion of the reaction by thin film chromatography, the reaction container was cooled with water. The formed crystals were separated by filtration and dissolved in 100 ml of hot ethanol. Insoluble materials were separated by filtration, and the filtrate was cooled. The resulting colorless crystals were Compound (1). The melting point was 182° to 185° C. and the yield was 12 g.

Aufarbeitung

  1. temperatureThe solution was refluxed
  2. temperaturewith heating
  3. customthe conclusion of the reaction by thin film chromatography
  4. customThe formed crystals were separated by filtration
  5. dissolutiondissolved in 100 ml of hot ethanol
  6. customInsoluble materials were separated by filtration
  7. temperaturethe filtrate was cooled

Quellen und Nachweise

ORD-Eintrag
ord-1bce0b5d3aca4363bf329d0a4059a7a2
Quelldatensatz
uspto-grants-1981_04
Patentnummer
US04264723

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