Acetic Acid → HCID 178508982, Verbindung

HRID 2372302Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 2372302
O.[NH2:2][C:3]1[N:8]=[C:7]([OH:9])[CH:6]=[C:5](Cl)[N:4]=1.[S:11]1[CH:15]=[CH:14][CH:13]=[C:12]1[CH2:16][NH2:17].C(N(CC)CC)C.C(O)(=O)C>COC(O)C>[NH2:2][C:3]1[N:8]=[C:7]([OH:9])[CH:6]=[C:5]([NH:17][CH2:16][C:12]2[S:11][CH:15]=[CH:14][CH:13]=2)[N:4]=1

Komponenten

6

Edukt 4

HCID 176Acetic AcidHCID 8471TriethylamineHCID 34005(2-Thienylmethyl)amineHCID 178508975HCID 178508975, Verbindung

Produkt 1

HCID 178508982HCID 178508982, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 30156371-MethoxyethanolLösungsmittel

Versuchsvorschrift

2-Amino-6-chloro-4-pyrimidinol, monohydrate (85%, 100 g, 0.5197 mol) was suspended in methoxyethanol (700 ml) and 2-thienylmethylamine (96%, 61.3 g, 0.5197 mol) was added to the suspension. The mixture was heated under reflux for two hours and then 73 ml (d =0.726; 0.52 mol) of triethylamine was added and the refluxing continued for an additional 18 hours. The reaction mixture was poured into ice water (1000 ml), acidified with acetic acid (ph 4.0) and the precipitated solid was filtered, washed, and dried. Yield: 110 g (72.6%). This was used in the next step without further purification.

Aufarbeitung

  1. temperatureThe mixture was heated
  2. temperatureunder reflux for two hours
  3. filtrationthe precipitated solid was filtered
  4. washwashed
  5. customdried
  6. customThis was used in the next step without further purification

Quellen und Nachweise

ORD-Eintrag
ord-defb3644829b4707896faf39697c8509
Quelldatensatz
uspto-grants-1992_03
Patentnummer
US05098905

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