Dimethylformamide → 2-(Acetoxymethyl)-5-[[bis(allyloxy)phosphoryl]oxymethyl]benzoyl chloride

HRID 1766860Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1766860
[C:1]([O:4][CH2:5][C:6]1[CH:14]=[CH:13][C:12]([CH2:15][O:16][P:17]([O:23][CH2:24][CH:25]=[CH2:26])([O:19][CH2:20][CH:21]=[CH2:22])=[O:18])=[CH:11][C:7]=1[C:8](O)=[O:9])(=[O:3])[CH3:2].C(Cl)(=O)C([Cl:30])=O.CN(C)C=O>O1CCCC1>[C:1]([O:4][CH2:5][C:6]1[CH:14]=[CH:13][C:12]([CH2:15][O:16][P:17]([O:23][CH2:24][CH:25]=[CH2:26])([O:19][CH2:20][CH:21]=[CH2:22])=[O:18])=[CH:11][C:7]=1[C:8]([Cl:30])=[O:9])(=[O:3])[CH3:2]

Komponenten

5

Edukt 3

HCID 6228DimethylformamideHCID 65578Oxalyl chlorideHCID 211104382-(Acetoxymethyl)-5-[[bis(allyloxy)phosphoryl]oxymethyl]benzoic acid

Produkt 1

HCID 178626372-(Acetoxymethyl)-5-[[bis(allyloxy)phosphoryl]oxymethyl]benzoyl chloride

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 8028TetrahydrofuranLösungsmittel

Reaktionsbedingungen

Temperatur
0 °C

Versuchsvorschrift

2-(Acetoxymethyl)-5-[[bis(allyloxy)phosphoryl]oxymethyl]benzoic acid (475.5 mg, 1.24 mmol) obtained from Example 1-(11) was dissolved in tetrahydrofuran (5 ml), and the solution was cooled to 0° C., then oxalyl chloride (189.2 mg, 1.49 mmol) and N,N-dimethylformamide (15 μl) were added thereto with stirring. The mixture was warmed to room temperature and then stirred for 40 minutes. The solvent was distilled off under reduced pressure to give the crude 2-(acetoxymethyl)-5-[[bis(allyloxy)phosphoryl]oxymethyl]benzoyl chloride.

Aufarbeitung

  1. temperatureThe mixture was warmed to room temperature
  2. stirringstirred for 40 minutes
  3. distillationThe solvent was distilled off under reduced pressure

Quellen und Nachweise

ORD-Eintrag
ord-6db3acf9bea14bda995306ee62c393c1
Quelldatensatz
uspto-grants-2007_06
Patentnummer
US07230023B2

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