(6,7-Difluoro-3-methyl-1,2-benzisoxazol-5-yl)methanol → HCID 86658113, Verbindung

HRID 245508Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 245508
[F:1][C:2]1[C:11]([CH2:12][OH:13])=[CH:10][C:5]2[C:6]([CH3:9])=[N:7][O:8][C:4]=2[C:3]=1[F:14]>C(Cl)Cl.[O-2].[O-2].[Mn+4].O=[Mn]=O>[F:1][C:2]1[C:11]([CH:12]=[O:13])=[CH:10][C:5]2[C:6]([CH3:9])=[N:7][O:8][C:4]=2[C:3]=1[F:14]

Komponenten

5

Edukt 1

HCID 67356869(6,7-Difluoro-3-methyl-1,2-benzisoxazol-5-yl)methanol2×

Produkt 1

HCID 86658113HCID 86658113, VerbindungAusbeute 92,5 %

Reagenzien, Katalysatoren, Lösungsmittel 3

HCID 14801Manganese dioxideKatalysatorHCID 178418406HCID 178418406, VerbindungKatalysatorHCID 6344DichloromethaneLösungsmittel

Versuchsvorschrift

A mixture of (6,7-difluoro-3-methyl-1,2-benzisoxazol-5-yl)methanol (Intermediate 334, 0.7 g, 3.51 mmol) and manganese dioxide (6.11 g, 70.30 mmol) in CH2Cl2 (70 ml) was stirred at room temperature for 3 days. TLC shows conversion to a higher Rf spot with starting material. Additional MnO2 (5 g) was added and the mixture was heated to reflux for 24 hours. The mixture was filtered through celite and rinsed well with CH2Cl2. Solvent was removed from the filtrate to give 640 mg of product as a tan solid.

Aufarbeitung

  1. temperaturethe mixture was heated
  2. temperatureto reflux for 24 hours
  3. filtrationThe mixture was filtered through celite
  4. washrinsed well with CH2Cl2
  5. customSolvent was removed from the filtrate

Quellen und Nachweise

ORD-Eintrag
ord-e75557fc1e6645f4924489f11d8a7053
Quelldatensatz
uspto-grants-2014_02
Patentnummer
US08658641B2

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