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Dimethylformamide → 4,4-Difluoro-3-methyl-3-butenyl 2-butoxy-4-methylpyrimidine-5-carboxylate

HRID 917371
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 917371
CN(C)C=O.CS([O:10][CH2:11][CH2:12][C:13]([CH3:17])=[C:14]([F:16])[F:15])(=O)=O.[CH2:18]([O:22][C:23]1[N:28]=[C:27]([CH3:29])[C:26]([C:30](O)=[O:31])=[CH:25][N:24]=1)[CH2:19][CH2:20][CH3:21].C(=O)([O-])O.[Na+]>O>[CH2:18]([O:22][C:23]1[N:28]=[C:27]([CH3:29])[C:26]([C:30]([O:10][CH2:11][CH2:12][C:13]([CH3:17])=[C:14]([F:16])[F:15])=[O:31])=[CH:25][N:24]=1)[CH2:19][CH2:20][CH3:21]
KomponentenReaktionsbedingungenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

6

Edukt 4

HCID 6228DimethylformamideHCID 516892Sodium BicarbonateHCID 230201272-Butoxy-4-methylpyrimidine-5-carboxylic acidHCID 230202374,4-Difluoro-3-Methyl-3-Buten-1-Yl Methanesulfonate

Produkt 1

HCID 691790234,4-Difluoro-3-methyl-3-butenyl 2-butoxy-4-methylpyrimidine-5-carboxylateAusbeute 32 %

Reagenzien, Katalysatoren, Lösungsmittel

1
HCID 962WaterLösungsmittel

Reaktionsbedingungen

Temperatur
100 °C

Versuchsvorschrift

To 50 ml of N,N-dimethylformamide were dissolved 6.6 g (33 mmol) of 4,4-difluoro-3-methyl-3-butenyl methanesulfonate and 7.6 g (36 mmol) of 2-butoxy-4-methylpyrimidine-5-carboxylic acid, followed by the addition of 3.6 g (43 mmol) of sodium hydrogencarbonate and stirring at 100° C. for 2 hours. The reaction liquid was then poured in water and extracted with ethyl acetate. The organic layer was washed with water and a saturated saline solution in this order, followed by drying over anhydrous magnesium sulfate and concentration under reduced pressure. The residue was purified with silica gel column chromatography (ethyl acetate:hexane=1:9) to obtain 3.3 g (yield: 32%) of 4,4-difluoro-3-methyl-3-butenyl 2-butoxy-4-methylpyrimidine-5-carboxylate.

Aufarbeitung

  1. customThe reaction liquid
  2. extractionextracted with ethyl acetate
  3. washThe organic layer was washed with water
  4. dry with materialby drying over anhydrous magnesium sulfate and concentration under reduced pressure
  5. customThe residue was purified with silica gel column chromatography (ethyl acetate:hexane=1:9)

Quellen und Nachweise

ORD-Eintrag
ord-e805e709080b4b0c9f156d88adde612e
Quelldatensatz
uspto-grants-2007_09
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US07273878B2

Notizen zur Reaktion

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