Triethylamine → HCID 178456876, Verbindung

HRID 1580591Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1580591
Cl.[NH2:2][C:3]([CH3:16])([CH3:15])[C:4](=[N:13][OH:14])[CH2:5][O:6][C:7]1[CH:12]=[CH:11][CH:10]=[CH:9][CH:8]=1.[NH2:17][C:18]1[N:23]=[C:22](Cl)[C:21]([N+:25]([O-:27])=[O:26])=[C:20]([OH:28])[N:19]=1.C(N(CC)CC)C>C(O)C>[NH2:17][C:18]1[N:19]=[C:20]([OH:28])[C:21]([N+:25]([O-:27])=[O:26])=[C:22]([NH:2][C:3]([CH3:16])([CH3:15])[C:4](=[N:13][OH:14])[CH2:5][O:6][C:7]2[CH:8]=[CH:9][CH:10]=[CH:11][CH:12]=2)[N:23]=1

Komponenten

5

Edukt 3

HCID 8471TriethylamineHCID 867329813-Amino-1-phenoxy-3-methylbutan-2-one oxime hydrochlorideHCID 178418667HCID 178418667, Verbindung

Produkt 1

HCID 178456876HCID 178456876, VerbindungAusbeute 16,1 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 702EthanolLösungsmittel

Versuchsvorschrift

A mixture of 3-amino-1-(p-chloro)-phenoxy-3-methylbutan-2-one oxime hydrochloride (IV) (5.58 g), 2-amino-4-chloro-6-hydroxy-5-nitropyrimidine (III) (Hal = Cl) (3.81 g) and dry triethylamine (8.2 g) was heated to reflux in dry ethanol (240 ml) for 16 hours and filtered hot. The filtrate was reduced in volume and the solid so obtained was filtered off. Recrystallisation from ethanol gave the nitropyrimidine oxime (II) (1.17 g) as a pale yellow gelatinous solid, m.p. >250°C (decomp.).

Aufarbeitung

  1. temperaturewas heated
  2. filtrationfiltered hot
  3. customthe solid so obtained
  4. filtrationwas filtered off
  5. customRecrystallisation from ethanol

Quellen und Nachweise

ORD-Eintrag
ord-d130ce69d23d49ad873b00c5c03e6964
Quelldatensatz
uspto-grants-1976_01
Patentnummer
US03933820

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