Benzene → 5-Acetoxy-2-(3-methoxymethoxypropyl)-4,6,7-trimethyl-1,3-benzoxathiole

HRID 2308877Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 2308877
[OH:1][C:2]1[C:3]([CH3:20])=[C:4]([CH3:19])[C:5]2[O:9][CH:8]([CH2:10][CH2:11][CH2:12][O:13][CH2:14][O:15][CH3:16])[S:7][C:6]=2[C:17]=1[CH3:18].[C:21](OC(=O)C)(=[O:23])[CH3:22].C1C=CC=CC=1>N1C=CC=CC=1>[C:21]([O:1][C:2]1[C:3]([CH3:20])=[C:4]([CH3:19])[C:5]2[O:9][CH:8]([CH2:10][CH2:11][CH2:12][O:13][CH2:14][O:15][CH3:16])[S:7][C:6]=2[C:17]=1[CH3:18])(=[O:23])[CH3:22]

Komponenten

5

Edukt 3

HCID 241BenzeneHCID 7918Acetic AnhydrideHCID 148021895-Hydroxy-2-(3-methoxymethoxypropyl)-4,6,7-trimethyl-1,3-benzoxathiole

Produkt 1

HCID 148021905-Acetoxy-2-(3-methoxymethoxypropyl)-4,6,7-trimethyl-1,3-benzoxathiole

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 1049PyridineLösungsmittel

Versuchsvorschrift

100 mg of 5-hydroxy-2-(3-methoxymethoxypropyl)-4,6,7-trimethyl-1,3-benzoxathiole (prepared as described in Example 83) were dissolved in 1 ml of pyridine, and 50 mg of acetic anhydride were added. The reaction mixture was allowed to react for 20 hours at room temperature. Benzene was then added to the reaction mixture, and the benzene solution was washed with water and then dried over anhydrous sodium sulfate. The benzene was distilled off under reduced pressure. The resulting residue was subjected to silica gel column chromatography. The title compound was obtained from the fraction eluted with a 20:1 by volume mixture of benzene and ethyl acetate.

Aufarbeitung

  1. customto react for 20 hours at room temperature
  2. washthe benzene solution was washed with water
  3. dry with materialdried over anhydrous sodium sulfate
  4. distillationThe benzene was distilled off under reduced pressure

Quellen und Nachweise

ORD-Eintrag
ord-d6ade16802ec4b11ab42ee4907a6d1e6
Quelldatensatz
uspto-grants-1987_09
Patentnummer
US04691027

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