N,N-Dimethylaniline → HCID 69250913, Verbindung
Reaktionsgleichung
[OH:1][CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][O:8][C:9]1[CH:17]=[CH:16][C:12]([C:13]([OH:15])=[O:14])=[C:11]([F:18])[CH:10]=1.CN(C)[C:21]1[CH:26]=[CH:25][CH:24]=[CH:23][CH:22]=1.[O:28]1C[CH2:31][CH2:30][CH2:29]1.C(Cl)(=O)C=C>C(C1C(O)=C(CCCC)C=C(C)C=1)CCC.O>[C:29]([CH2:22][CH2:23][CH2:24][CH2:25][CH2:26][CH2:21][O:1][CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][O:8][C:9]1[CH:17]=[CH:16][C:12]([C:13]([OH:15])=[O:14])=[C:11]([F:18])[CH:10]=1)(=[O:28])[CH:30]=[CH2:31]Komponenten
7
Edukt 4
Produkt 1
Reagenzien, Katalysatoren, Lösungsmittel 2
Reaktionsbedingungen
- Temperatur
- 60 °C
Versuchsvorschrift
Under a nitrogen atmosphere, 4-(6-hydroxyhexyloxy)-2-fluorobenzoic acid (189 g), N,N-dimethylaniline (133 g) and 2,6-dibutyl-p-cresol (0.80 g) were added to tetrahydrofuran (500 mL). Acrylic acid chloride (100 g) was added dropwise thereto, followed by agitating at 60° C. for 3 hours. The reaction solution was poured into water and extracted with ethyl acetate. The organic layer was washed with hydrochloric acid, a saturated sodium hydrogencarbonate aqueous solution and water, and after drying over anhydrous magnesium sulfate, the solvent was distilled off under reduced pressure. The resulting residue was recrystallized from ethanol to obtain 4-(6-acryloylhexyloxyhexyloxy)-2-fluorobenzoic acid (141 g).
Aufarbeitung
- extractionextracted with ethyl acetate
- washThe organic layer was washed with hydrochloric acid
- dry with materiala saturated sodium hydrogencarbonate aqueous solution and water, and after drying over anhydrous magnesium sulfate
- distillationthe solvent was distilled off under reduced pressure
- customThe resulting residue was recrystallized from ethanol
Quellen und Nachweise
- ORD-Eintrag
- ord-ca72d716246f4bfab9b90c9e30af08c1
- Quelldatensatz
- uspto-grants-2008_05
- Patentnummer
- US07378135B2
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