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Sulfuric Acid → HCID 69735150, Verbindung

HRID 1814608
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1814608
[Br:1][C:2]1[CH:15]=[CH:14][C:5]([C:6]([C:8]2[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=2)=O)=[CH:4][CH:3]=1.C(OP([CH2:24][C:25]1[CH:30]=[C:29]([O:31][CH3:32])[C:28]([CH2:33]P(OCC)(OCC)=O)=[CH:27][C:26]=1[O:42][CH2:43][CH:44]([CH2:49][CH3:50])[CH2:45][CH2:46][CH2:47][CH3:48])(OCC)=O)C.[C:51](O[K])([CH3:54])([CH3:53])[CH3:52].S(=O)(=O)(O)O>O1CCCC1.C(OCC)(=O)C.O>[Br:1][C:2]1[CH:15]=[CH:14][C:5]([C:6]([C:8]2[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=2)=[CH:24][C:25]2[CH:30]=[C:29]([O:31][CH3:32])[C:28]([CH:33]=[C:52]([C:8]3[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=3)[C:51]3[CH:54]=[CH:15][C:2]([Br:1])=[CH:3][CH:53]=3)=[CH:27][C:26]=2[O:42][CH2:43][CH:44]([CH2:49][CH3:50])[CH2:45][CH2:46][CH2:47][CH3:48])=[CH:4][CH:3]=1
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

8

Edukt 4

HCID 1118Sulfuric AcidHCID 70304-BromobenzophenoneHCID 58887345HCID 58887345, VerbindungHCID 178418922HCID 178418922, Verbindung

Produkt 1

HCID 69735150HCID 69735150, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 3

HCID 962
Water
Lösungsmittel
HCID 8028TetrahydrofuranLösungsmittel2×
HCID 8857Ethyl AcetateLösungsmittel

Versuchsvorschrift

Under an inert atmosphere, 4-bromobenzophenone (0.783 g, 3mmol), and 1,4-bis-(diethylphosphonomethyl)-2-(2-ethylhexyloxy)-5-methoxy benzene (0.660 g, 1.23 mmol) were dissolved in tetrahydrofuran (10 g). At room temperature, tetrahydrofuran (3.28 g) solution of tert-butoxy potassium (0.414 g, 3.69 mmol) was added dropwise for 5 minutes, and successively stirred for 3.5 hours. The reaction mixture was charged into water (100 ml) and neutralized with 5% sulfuric acid. After neutralization, ethyl acetate (250 ml) was added and the organic layer was partitioned. The organic layer was washed with water and dried over anhydrous sodium sulfate. The solvent was distilled off under reduced pressure, and the resultant raw product was purified by silica gel chromatography to give the desired product. (Yield: 0.86 g, 93%)

Aufarbeitung

  1. customthe organic layer was partitioned
  2. washThe organic layer was washed with water
  3. dry with materialdried over anhydrous sodium sulfate
  4. distillationThe solvent was distilled off under reduced pressure
  5. customthe resultant raw product was purified by silica gel chromatography

Quellen und Nachweise

ORD-Eintrag
ord-f1ad3f57de03421082d4a0d31ddd2a74
Quelldatensatz
uspto-grants-2005_04
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US06875895B2

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