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Bromine → HCID 86723840, Verbindung

HRID 576741
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Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 576741
[F:1][C:2]([F:18])([F:17])[C:3]1[CH:4]=[C:5]([N:9]2[CH2:14][CH2:13][C:12](=[O:15])[NH:11][C:10]2=[O:16])[CH:6]=[CH:7][CH:8]=1.BrBr.S([O-])([O-])(=O)=S.[Na+].[Na+].[Br:28][C:29]1[C:30](=[O:46])[NH:31][C:32](=[O:45])[N:33]([C:35]2[CH:40]=[CH:39][CH:38]=[C:37]([C:41]([F:44])([F:43])[F:42])[CH:36]=2)[CH:34]=1.BrC1(Br)CN(C2C=CC=C(C(F)(F)F)C=2)C(=O)NC1=O.BrC1CN(C2C=CC=C(C(F)(F)F)C=2)C(=O)NC1=O.[Cl-].[Li+]>C(O)(=O)C.CN(C)C=O.O>[Br:28][C:29]1[C:30](=[O:46])[NH:31][C:32](=[O:45])[N:33]([C:35]2[CH:40]=[CH:39][CH:38]=[C:37]([C:41]([F:44])([F:43])[F:42])[CH:36]=2)[CH:34]=1.[F:18][C:2]([F:1])([F:17])[C:3]1[CH:4]=[C:5]([N:9]2[CH:14]=[CH:13][C:12](=[O:15])[NH:11][C:10]2=[O:16])[CH:6]=[CH:7][CH:8]=1
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

12

Edukt 7

HCID 24408BromineHCID 24477Sodium ThiosulfateHCID 433294Lithium ChlorideHCID 70692250HCID 70692250, VerbindungHCID 86723840HCID 86723840, VerbindungHCID 86723842HCID 86723842, Verbindung
HCID 86723843
HCID 86723843, Verbindung

Produkt 2

HCID 86723840HCID 86723840, VerbindungHCID 86723841HCID 86723841, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 3

HCID 176Acetic AcidLösungsmittelHCID 962WaterLösungsmittel2×HCID 6228DimethylformamideLösungsmittel

Versuchsvorschrift

To a solution of 1-(3-trifluoromethylphenyl)dihydropyrimidin-2,4(1H,3H)-dione (prepared in Reference Example 96) (770.0 mg) in acetic acid (10.0 ml) was added bromine (0.18 ml) and the resulting mixture was stirred with heating under reflux for two hours. To the reaction mixture were added water (30 ml) and 10% aqueous sodium thiosulfate solution (5 ml) and the precipitated solids were collected by filtration with water to afford a mixture containing 5-bromo-1-(3-trifluoromethylphenyl)pyrimidin-2,4(1H,3H)-dione, 5,5-dibromo-1-(3-trifluoromethylphenyl)dihydropyrimidin-2,4(1H,3H)-dione and 5-bromo-1-(3-trifluoromethylphenyl)dihydropyrimidin-2,4(1H,3H)-dione (800.0 mg). A solution of the resulting mixture (800.0 mg) and lithium chloride (122.3 mg) in N,N-dimethyl formamide (5.0 ml) was stirred at 120° C. for one and a half hours. To the reaction mixture was added water (20 ml) and the resulting mixture was extracted with ethyl acetate (20 ml×2), and the organic layer was washed with water (20 ml×2) and saturated saline (20 ml), dried over anhydrous sodium sulfate and then concentrated under reduced pressure. The residue was purified by silica gel column chromatography (eluent: hexane/ethyl acetate) to afford 5-bromo-1-(3-trifluoromethylphenyl)pyrimidin-2,4(1H,3H)-dione (473.1 mg) and 1-(3-trifluoromethylphenyl)pyrimidin-2,4(1H,3H)-dione (135.8 mg).

Aufarbeitung

  1. temperaturewith heating
  2. temperatureunder reflux for two hours
  3. filtrationthe precipitated solids were collected by filtration with water
  4. customto afford a mixture
  5. extractionthe resulting mixture was extracted with ethyl acetate (20 ml×2)
  6. washthe organic layer was washed with water (20 ml×2) and saturated saline (20 ml)
  7. dry with materialdried over anhydrous sodium sulfate
  8. concentrationconcentrated under reduced pressure
  9. customThe residue was purified by silica gel column chromatography (eluent: hexane/ethyl acetate)

Quellen und Nachweise

ORD-Eintrag
ord-7ca61d9bd7a843c98a1ea492b47c803d
Quelldatensatz
uspto-grants-2015_05
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US09040516B2

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