Hydrochloric Acid → HCID 178439570, Verbindung

HRID 463360

Reaktionsgleichung

Reaktionsgleichung von HRID 463360
[C:1]([C:3]([NH:8][C:9](=O)[C:10]1[C:11](=[CH:15][CH:16]=[CH:17][CH:18]=1)[C:12]([OH:14])=[O:13])([CH3:7])[CH:4]([CH3:6])[CH3:5])#[N:2].[OH-:20].[Na+].OO.[ClH:24]>C(O)(C)C.O>[ClH:24].[CH:4]([C:3]1([CH3:7])[NH:8][C:9]([C:10]2[CH:18]=[CH:17][CH:16]=[CH:15][C:11]=2[C:12]([OH:14])=[O:13])=[N:2][C:1]1=[O:20])([CH3:6])[CH3:5]

Komponenten

7

Edukt 4

HCID 313Hydrochloric AcidHCID 784Hydrogen PeroxideHCID 14798Sodium HydroxideHCID 4890749N-(cyano-1,2-dimethylpropyl)phthalamic acid

Produkt 1

HCID 178439570HCID 178439570, VerbindungAusbeute 60,3 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 962WaterLösungsmittelHCID 3776IsopropanolLösungsmittel

Reaktionsbedingungen

Temperatur
80 °C

Versuchsvorschrift

To 5.22 g (0.020 mol) of N-(1-cyano-1,2-dimethylpropyl)phthalamic acid in a mixture of 35 mL isopropyl alcohol and 10 mL of water is added 6.41 g (0.080 mol) of aqueous 50% sodium hydroxide. External cooling is applied to hold the temperature at 20°-30° C. and 4.80 g (0.042 mol) of aqueous 30% hydrogen peroxide is added. The mixture is heated at 80° C. for five hours then cooled to 20°-25° C. Aqueous 36% hydrochloric acid is added to adjust the pH to 1. The volatile solvent is removed in vacuo to give 8.35 g of solid 2-(5-isopropyl-5-methyl-4-oxo-2-imidazolin-2-yl)benzoic acid, hydrochloride salt. The solid is analyzed by high performance liquid chromatography. The real yield is 60.3%.

Aufarbeitung

  1. temperatureExternal cooling
  2. customat 20°-30° C.
  3. temperaturethen cooled to 20°-25° C
  4. customThe volatile solvent is removed in vacuo

Quellen und Nachweise

ORD-Eintrag
ord-4ee2aaf424bd413a900cac62420d4ab2
Quelldatensatz
uspto-grants-1985_05
Patentnummer
US04518780

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