Toluene → HCID 24855179, Verbindung

HRID 452585Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 452585
[C:1]1([CH:7]2[S:12][CH2:11][CH2:10][NH:9][CH2:8]2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.Cl[C:14]1[C:23]2[C:18](=[CH:19][C:20]([O:26][CH3:27])=[C:21]([O:24][CH3:25])[CH:22]=2)[N:17]=[CH:16][N:15]=1.C(=O)([O-])[O-].[K+].[K+].C1(C)C=CC=CC=1>CC(O)C>[CH3:25][O:24][C:21]1[CH:22]=[C:23]2[C:18](=[CH:19][C:20]=1[O:26][CH3:27])[N:17]=[CH:16][N:15]=[C:14]2[N:9]1[CH2:10][CH2:11][S:12][CH:7]([C:1]2[CH:2]=[CH:3][CH:4]=[CH:5][CH:6]=2)[CH2:8]1

Komponenten

6

Edukt 4

HCID 1140TolueneHCID 11430Potassium CarbonateHCID 27693644-Chloro-6,7-dimethoxyquinazolineHCID 50041992-phenylthiomorpholine

Produkt 1

HCID 24855179HCID 24855179, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 3776IsopropanolLösungsmittel

Reaktionsbedingungen

Temperatur
180 °C

Versuchsvorschrift

2-Phenyl-thiomorpholine (1 mole equivalent), 4-Chloro-6,7-dimethoxy-quinazoline (1 mole equivalent) and potassium carbonate (1 mole equivalent) were added to a 1:1 mixture of toluene and 2-propanol, corresponding to a final concentration of about 0.5 molar. The reaction mixture was heated in a microwave oven at 180° C. for 15 minutes, and filtrated. The solvent was removed under vacuum and the resultant solid was subjected to preparative LC-MS-purification. Fractions containing the product were collected, pooled and evaporated in vacuo to give the product.

Aufarbeitung

  1. filtrationfiltrated
  2. customThe solvent was removed under vacuum
  3. additionFractions containing the product
  4. customwere collected
  5. customevaporated in vacuo
  6. customto give the product

Quellen und Nachweise

ORD-Eintrag
ord-e3fbcc95693f48cda2fa4a33eb313089
Quelldatensatz
uspto-grants-2013_07
Patentnummer
US08492394B2

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