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Trichloroisocyanuric Acid → HCID 20544433, Verbindung

HRID 2285842
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 2285842
[O:1]=[C:2]1[CH:7]=[C:6]([CH2:8][OH:9])[NH:5][CH:4]=[C:3]1[O:10][CH2:11][C:12]([OH:14])=[O:13].[Cl:15]N1C(=O)N(Cl)C(=O)N(Cl)C1=O>CO.O>[O:1]=[C:2]1[C:7]([Cl:15])=[C:6]([CH2:8][OH:9])[NH:5][CH:4]=[C:3]1[O:10][CH2:11][C:12]([OH:14])=[O:13]
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

5

Edukt 2

HCID 6909Trichloroisocyanuric AcidHCID 20544454HCID 20544454, Verbindung

Produkt 1

HCID 20544433HCID 20544433, VerbindungAusbeute 121,2 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 887MethanolLösungsmittelHCID 962WaterLösungsmittel

Versuchsvorschrift

2-(4-Oxo-6-hydroxymethyl-1,4-dihydropyridin-3-yloxy)acetic acid (5.97 g) was dissolved in a mixture of methanol (300 ml) and water (420 ml) at 65° to 70° C. and the solution was stirred at the same temperature. Trichloroisocyanuric acid (2.79 g) was added thereto, and the resultant mixture was stirred at the same temperature for 1.5 hours and then allowed to stand at room temperature over-night. The reaction mixture was cooled and the resulting crystals were collected by filtration, washed with water and dried. Thus obtained crystals (4.1 g) were recrystallized from water (100 ml) to give crystals (3.4 g) of 2-(4-oxo-5-chloro-6-hydroxymethyl-1,4-dihydropyridin-3-yloxy) acetic acid, mp 240° to 245° C.(dec).

Aufarbeitung

  1. waitto stand at room temperature over-night
  2. temperatureThe reaction mixture was cooled
  3. filtrationthe resulting crystals were collected by filtration
  4. washwashed with water
  5. customdried
  6. customThus obtained crystals (4.1 g) were recrystallized from water (100 ml)

Quellen und Nachweise

ORD-Eintrag
ord-0bed78c286184b4ca7b48398e83d44fd
Quelldatensatz
uspto-grants-1982_04
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US04324892

Notizen zur Reaktion

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