Water → HCID 70288966, Verbindung

HRID 377757

Reaktionsgleichung

Reaktionsgleichung von HRID 377757
[F:1][C:2]1[CH:3]=[C:4]2[C:8](=[CH:9][C:10]=1[F:11])[CH2:7][C:6]([CH3:12])=[C:5]2[CH2:13][C:14]([O:16]C)=[O:15].[CH3:18][S:19]([C:22]1[CH:29]=[CH:28][C:25]([CH:26]=O)=[CH:24][CH:23]=1)(=[O:21])=[O:20].O>N1C=CC=CC=1>[F:1][C:2]1[CH:3]=[C:4]2[C:8](=[CH:9][C:10]=1[F:11])/[C:7](=[CH:26]\[C:25]1[CH:24]=[CH:23][C:22]([S:19]([CH3:18])(=[O:21])=[O:20])=[CH:29][CH:28]=1)/[C:6]([CH3:12])=[C:5]2[CH2:13][C:14]([OH:16])=[O:15]

Komponenten

5

Edukt 3

HCID 962Water2×HCID 2203764-(Methylsulfonyl)benzaldehydeHCID 12052144HCID 12052144, Verbindung

Produkt 1

HCID 70288966HCID 70288966, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 1049PyridineLösungsmittel

Versuchsvorschrift

Methyl 5,6-difluoro-2-methylindene-3-acetate (1.19 g, 5.0 mmol) from Example 2, Part E and of p-methylsulfonylbenzaldehyde (0.76 g, 5.0 mmol) in dry pyridine (10 ml) are treated under nitrogen with Triton B (5.0 g, 5.1 mmol). The deeply colored solution is kept overnight. Water (2 ml) is added, the solution is stirred for 15 minutes and is poured into excess water. The mixture is extracted with ether (2×50 ml). The aqueous phase is added to 10% HCl-ice. The solution of the precipitate is extracted into methylene chloride and is dried (MgSO4). The solvent is evaporated to leave an orange solid which is recrystallized from benzene to give (Z)-5,6-difluoro-2-methyl-1-(p-methylsulfonylbenzylidene)-indene-3-acetic acid.

Aufarbeitung

  1. extractionThe mixture is extracted with ether (2×50 ml)
  2. additionThe aqueous phase is added to 10% HCl-ice
  3. extractionThe solution of the precipitate is extracted into methylene chloride
  4. dry with materialis dried (MgSO4)
  5. customThe solvent is evaporated
  6. customto leave an orange solid which
  7. customis recrystallized from benzene

Quellen und Nachweise

ORD-Eintrag
ord-5f0ad651339a4210bcd234822b133a3f
Quelldatensatz
uspto-grants-2000_02
Patentnummer
US06028116

Verknüpfte Notizen

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