Hydrochloric Acid → HCID 178481601, Verbindung

HRID 33964

Reaktionsgleichung

Reaktionsgleichung von HRID 33964
[CH3:1][N:2]1[C:7](=[O:8])[C:6]([C:9]2[CH:18]=[CH:17][C:16]3[C:11](=[CH:12][CH:13]=[CH:14][CH:15]=3)[CH:10]=2)=[C:5]([C:19]2[CH:24]=[CH:23][N:22]=[CH:21][CH:20]=2)[N:4]=[C:3]1SC.C(Cl)Cl.C[OH:31].Cl>O1CCOCC1.[OH-].[Na+]>[OH:31][C:3]1[N:2]([CH3:1])[C:7](=[O:8])[C:6]([C:9]2[CH:18]=[CH:17][C:16]3[C:11](=[CH:12][CH:13]=[CH:14][CH:15]=3)[CH:10]=2)=[C:5]([C:19]2[CH:24]=[CH:23][N:22]=[CH:21][CH:20]=2)[N:4]=1

Komponenten

6

Edukt 3

HCID 313Hydrochloric AcidHCID 21226129Dichloromethane methanolHCID 223466413-methyl-2-methylsulfanyl-5-naphthalen-2-yl-6-pyridin-4-yl-3H-pyrimidin-4-one

Produkt 1

HCID 178481601HCID 178481601, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 14798Sodium HydroxideLösungsmittelHCID 312751,4-DioxaneLösungsmittel

Versuchsvorschrift

A suspension of 3-methyl-2-methylsulfanyl-5-naphthalen-2-yl-6-pyridin-4-yl-3H-pyrimidin-4-one (10.1 g, 28.1 mmol) was heated to 100° C. in 100 mL 1,4-dioxane and 60 mL 2.5M sodium hydroxide. After 7 h, TLC (95:5 DCM/MeOH) shows the solution to have no remaining starting material. The reaction was cooled to room temperature and acidified to pH 5 with 5M HCl. The resulting precipitate was collected by filtration, and then suspended in 100 mL hot methanol. The solid was cooled to room temperature then collected by filtration and washed with 100 mL diethylether. The product was air dried overnight to give a pale yellow solid. M+1=330.2.

Aufarbeitung

  1. filtrationThe resulting precipitate was collected by filtration
  2. temperatureThe solid was cooled to room temperature
  3. filtrationthen collected by filtration
  4. washwashed with 100 mL diethylether
  5. customdried overnight
  6. customto give a pale yellow solid

Quellen und Nachweise

ORD-Eintrag
ord-4dcf350333074a329c3813bb192a0da1
Quelldatensatz
uspto-grants-2008_09
Patentnummer
US07429594B2

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