Hydrochloric Acid → HCID 12138358, Verbindung

HRID 1271668Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1271668
[C:1]([C:5]1[CH:6]=[C:7]([CH:36]=[C:37]([C:39]([CH3:42])([CH3:41])[CH3:40])[CH:38]=1)[CH2:8][S:9][C:10]1[CH:11]=[C:12]([CH:17]=[C:18]([S:20][CH2:21][C:22]2[CH:27]=[C:26]([C:28]([CH3:31])([CH3:30])[CH3:29])[CH:25]=[C:24]([C:32]([CH3:35])([CH3:34])[CH3:33])[CH:23]=2)[CH:19]=1)[C:13](OC)=[O:14])([CH3:4])([CH3:3])[CH3:2].Cl>C1(C)C=CC=CC=1>[C:32]([C:24]1[CH:23]=[C:22]([CH:27]=[C:26]([C:28]([CH3:31])([CH3:30])[CH3:29])[CH:25]=1)[CH2:21][S:20][C:18]1[CH:17]=[C:12]([CH:11]=[C:10]([S:9][CH2:8][C:7]2[CH:6]=[C:5]([C:1]([CH3:2])([CH3:3])[CH3:4])[CH:38]=[C:37]([C:39]([CH3:42])([CH3:41])[CH3:40])[CH:36]=2)[CH:19]=1)[CH2:13][OH:14])([CH3:35])([CH3:33])[CH3:34]

Komponenten

4

Edukt 2

HCID 313Hydrochloric AcidHCID 12138357HCID 12138357, Verbindung

Produkt 1

HCID 12138358HCID 12138358, VerbindungAusbeute 10 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 1140TolueneLösungsmittel2×

Versuchsvorschrift

Methyl 3,5-bis(3,5-di-tertiary-butylbenzylthio)benzoate (52.0 g, 86.0 mmol) was dissolved in 300 ml of toluene. To this, was added dropwise a 70% solution of sodium dihydrobis(2-methoxyethoxy)aluminate in toluene (52 g, 180.0 mmol), maintaining the temperature at 35° C. or below and the resulting mixture was stirred for 2 hours under the same conditions. After completion of the reaction, the reaction mixture was poured into 500 ml of a cold 10% hydrochloric acid solution, followed by stirring for 10 minutes. The toluene layer was separated, dried over anhydrous magnesium sulfate and then concentrated. The resulting residue was then purified by means of chromatography with dichloromethane, giving 4.96 g of 3,5-bis(3,5-di-tertiary-butylbenzylthio)benzyl alcohol as a viscous substance.

Aufarbeitung

  1. temperaturemaintaining the temperature at 35° C. or below
  2. customAfter completion of the reaction
  3. stirringby stirring for 10 minutes
  4. customThe toluene layer was separated
  5. dry with materialdried over anhydrous magnesium sulfate
  6. concentrationconcentrated
  7. customThe resulting residue was then purified by means of chromatography with dichloromethane

Quellen und Nachweise

ORD-Eintrag
ord-5a614f9d2639440d97c3e78c96e425d4
Quelldatensatz
uspto-grants-2007_04
Patentnummer
US07205428B2

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