Water → HCID 86596089, Verbindung

HRID 507493Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 507493
[CH3:1][S:2]([C:5]1[CH:6]=[CH:7][C:8]([C@@H:11]([OH:21])[C@H:12]([NH:15][C:16]([CH:18]([Cl:20])[Cl:19])=[O:17])[CH2:13][F:14])=[CH:9][CH:10]=1)(=[O:4])=[O:3].[C:22]1(=[O:32])[O:27][C:25](=[O:26])[C:24]2=[CH:28][CH:29]=[CH:30][CH:31]=[C:23]12.C(N(CC)CC)C.[OH2:40]>O1CCOCC1.ClCCl>[CH3:1][S:2]([C:5]1[CH:6]=[CH:7][C:8]([C@@H:11]([OH:21])[C@H:12]([NH:15][C:16]([CH:18]([Cl:20])[Cl:19])=[O:17])[CH2:13][F:14])=[CH:9][CH:10]=1)(=[O:4])=[O:3].[C:25]([O-:27])(=[O:26])[C:24]1[C:23](=[CH:31][CH:30]=[CH:29][CH:28]=1)[C:22]([O-:32])=[O:40]

Komponenten

7

Edukt 4

HCID 962WaterHCID 6811Phthalic AnhydrideHCID 8471TriethylamineHCID 114811Florfenicol

Produkt 1

HCID 86596089HCID 86596089, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 6344DichloromethaneLösungsmittelHCID 312751,4-DioxaneLösungsmittel

Versuchsvorschrift

3.9 g of florfenicol, 3.6 g of phthalic anhydride and 7.2 ml of triethyl amine in 36 ml of dioxane were taken in a 100 ml round bottom flask equipped with a magnetic stir bar and a drying tube. The reaction mixture was stirred at room temperature for 6 hours. After 6 hours, the contents were poured into 300 ml of cold water. The resulting gummy solid was dissolved in dichloromethane and washed thoroughly with saturated bicarbonate several times followed by water. The organic layer was dried over anhydrous sodium sulfate and concentrated over roto-evaporator. The semisolid obtained was recrystallized in a mixture of ethylacetate and hexane to obtain a solid product of 4.2 grams.

Aufarbeitung

  1. customequipped with a magnetic stir bar and a drying tube
  2. waitAfter 6 hours
  3. washwashed thoroughly with saturated bicarbonate several times
  4. dry with materialThe organic layer was dried over anhydrous sodium sulfate
  5. concentrationconcentrated over roto-evaporator
  6. customThe semisolid obtained
  7. customwas recrystallized in a mixture of ethylacetate and hexane
  8. customto obtain a solid product of 4.2 grams

Quellen und Nachweise

ORD-Eintrag
ord-9fb5d09d966045bdb4f9a1d791fde57e
Quelldatensatz
uspto-grants-2010_08
Patentnummer
US07786167B2

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