2,3-Butanediol → HCID 57720059, Verbindung

HRID 1985592Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1985592
[CH3:1][CH:2]([OH:6])[CH:3]([OH:5])[CH3:4].[C:7]1([CH3:17])[CH:12]=[CH:11][C:10](S(O)(=O)=O)=[CH:9][CH:8]=1.[C:18]1(C)C=CC=CC=1>>[CH3:4][CH:3]1[CH:2]([CH3:1])[O:6][C:8]2([CH:9]([CH3:18])[CH2:10][CH2:11][CH2:12][CH:7]2[CH3:17])[O:5]1

Komponenten

4

Edukt 3

HCID 2622,3-ButanediolHCID 1140TolueneHCID 6101p-Toluenesulfonic acid

Produkt 1

HCID 57720059HCID 57720059, Verbindung

Reaktionsbedingungen

Temperatur
120 °C

Versuchsvorschrift

A reaction flask equipped with a Dean Stark trap was charged with 2,6-dimethyl cyclohehanone (200 g), 2,3-butanediol (315 g), p-toluenesulfonic acid (2 g) and toluene (300 mL). The reaction mass was heated to reflux (110-130° C.). Water (36 mL) was collected in the Dean Stark trap. When no water was recovered the reaction mass was cooled to an ambient temperature, neutralized with 10% aqueous sodium carbonate (100 mL) and washed with brine. Purification by vacuum distillation afforded 2,3,6,10-tetramethyl-1,4-dioxaspiro[4,5]decane (265 g)), which had a boiling point of 104° C. at a pressure of 16 mmHg.

Aufarbeitung

  1. customA reaction flask equipped with a Dean Stark trap
  2. temperatureThe reaction mass was heated
  3. customWater (36 mL) was collected in the Dean Stark trap
  4. customWhen no water was recovered the reaction mass
  5. temperaturewas cooled to an ambient temperature
  6. washwashed with brine
  7. customPurification
  8. distillationby vacuum distillation

Quellen und Nachweise

ORD-Eintrag
ord-1df32608bbf54058ade937eac99e49ac
Quelldatensatz
uspto-grants-2009_06
Patentnummer
US07547668B1

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