Hydrochloric Acid → 1-Bromo-4-(7-methoxyheptylthio)benzene

HRID 1977285

Reaktionsgleichung

Reaktionsgleichung von HRID 1977285
[Br:1][C:2]1[CH:7]=[CH:6][C:5]([S:8][CH2:9][CH2:10][CH2:11][CH2:12][CH2:13][CH2:14][CH2:15]Br)=[CH:4][CH:3]=1.[CH3:17][O-:18].[Na+].Cl>CO.CCC(C(OCCN1C(C)C(C2C=CC=CC=2)OCC1)=O)C1C=CC=CC=1>[Br:1][C:2]1[CH:7]=[CH:6][C:5]([S:8][CH2:9][CH2:10][CH2:11][CH2:12][CH2:13][CH2:14][CH2:15][O:18][CH3:17])=[CH:4][CH:3]=1

Komponenten

6

Edukt 3

HCID 313Hydrochloric AcidHCID 10942334Sodium MethoxideHCID 219974831-Bromo-4-(7-bromoheptylthio)benzene

Produkt 1

HCID 219975631-Bromo-4-(7-methoxyheptylthio)benzene

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 887MethanolLösungsmittelHCID 20395FenbutrazateLösungsmittel

Versuchsvorschrift

To a solution of 1-bromo-4-(7-bromoheptylthio)benzene (5 g) in methanol (25 ml) was added 28% sodium mehtylate in nethanol (7.9 g) and the mixture was stirred under refluxing for 2 hours. The residue was adjusted to pH 2 with dilute HCl aq. and extracted with ethyl acetate. The organic layer was seperated, wahsed with brine, dried over magnesium sulfate and evaporated under reduced pressure. The residue was purified by column chromatography on silica gel eluting with n-hexane/ethyl acetate (50:1) to give 1-bromo-4-(7-methoxyheptylthio)benzene (3.59 g).

Aufarbeitung

  1. temperatureunder refluxing for 2 hours
  2. extractionextracted with ethyl acetate
  3. customThe organic layer was seperated
  4. dry with materialdried over magnesium sulfate
  5. customevaporated under reduced pressure
  6. customThe residue was purified by column chromatography on silica gel eluting with n-hexane/ethyl acetate (50:1)

Quellen und Nachweise

ORD-Eintrag
ord-3922bb71b3ae40dc9c6c6221f25629ac
Quelldatensatz
uspto-grants-2001_05
Patentnummer
US06232290B1

Verknüpfte Notizen

Wird geladen…