Acetic Acid → HCID 178517892, Verbindung

HRID 1805993Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1805993
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([N:8]2[CH2:13][CH2:12][NH:11][CH2:10][CH2:9]2)=[CH:4][CH:3]=1.[C:14]([OH:17])(=O)[CH3:15].Cl[C:19]1[N:20]=C(NC2C=C(C=CC=2)C(O)=O)C2[S:27][CH2:26][CH2:25][C:23]=2[N:24]=1>O>[Cl:1][C:2]1[CH:3]=[CH:4][C:5]([N:8]2[CH2:13][CH2:12][N:11]([C:19]3[N:20]=[C:14]([OH:17])[C:15]4[S:27][CH2:26][CH2:25][C:23]=4[N:24]=3)[CH2:10][CH2:9]2)=[CH:6][CH:7]=1

Komponenten

5

Edukt 3

HCID 176Acetic AcidHCID 974781-(4-Chlorophenyl)piperazineHCID 576001073-(2-Chloro-6,7-dihydrothieno[3,2-d]pyrimidin-4-ylamino)benzoic acid

Produkt 1

HCID 178517892HCID 178517892, VerbindungAusbeute 96,1 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 962WaterLösungsmittel

Reaktionsbedingungen

Temperatur
180 °C

Versuchsvorschrift

1.9 g (9.66 mmol) of 1-(4-chlorophenyl)piperazine is placed in 0.55 mL (9.62 mmol) of glacial acetic acid and heated to 180° C. in the heating block. 0.800 g (3.73 mmol) of 2-ethylsulfanyl-6,7-dihydrothieno[3,2-d]pyrimidin-4-ol (I) is added, then the mixture is left to stand for 1.5 hours at 180° C. and 16 hours at ambient temperature. Then the reaction mixture is combined with water and treated in the ultrasound bath. The precipitate is suction filtered, washed, and dried. 1.25 g of product II is obtained and used further in the crude state.

Aufarbeitung

  1. waitthe mixture is left
  2. additiontreated in the ultrasound bath
  3. filtrationfiltered
  4. washwashed
  5. customdried

Quellen und Nachweise

ORD-Eintrag
ord-f0845963e50b4252917224014cbdd133
Quelldatensatz
uspto-grants-2013_01
Patentnummer
US08354531B2

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