Hydrochloric Acid → HCID 178447845, Verbindung

HRID 465288

Reaktionsgleichung

Reaktionsgleichung von HRID 465288
[CH2:1]([C@H:4]1[CH2:9][CH2:8][C@H:7]([CH:10]2[CH2:15][CH2:14][C:13](=[O:16])[CH2:12][CH2:11]2)[CH2:6][CH2:5]1)[CH2:2][CH3:3].[C:17]1([OH:23])[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=1.Cl.O>C1(C)C=CC=CC=1>[OH:16][C:13]1[CH:14]=[CH:15][C:10]([C:7]2([C:20]3[CH:21]=[CH:22][C:17]([OH:23])=[CH:18][CH:19]=3)[CH2:6][CH2:5][CH:4]([C@H:1]3[CH2:3][CH2:2][C@H:1]([CH2:4][CH2:5][CH3:6])[CH2:3][CH2:2]3)[CH2:9][CH2:8]2)=[CH:11][CH:12]=1

Komponenten

6

Edukt 4

HCID 313Hydrochloric AcidHCID 962WaterHCID 996PhenolHCID 178447904HCID 178447904, Verbindung

Produkt 1

HCID 178447845HCID 178447845, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 1140TolueneLösungsmittel

Versuchsvorschrift

4-(Trans-4-n-propylcyclohexyl)cyclohexanone (449 g), phenol (756 g) and CaCl (446 g) were mixed, followed by gradually dropwise adding conc. hydrochloric acid (335 ml) with vigorous stirring at room temperature, further agitating the mixture for 30 minutes after completion of the dropwise addition, allowing the resulting material to stand at room temperature, further for 50 hours, adding hot water (2 l) and toluene (3 l), heating the mixture, cooling, filtering off crystals, washing the crystals with water and then with toluene, drying the crystals and recrystallizing from tetrahydrofuran solvent to obtain white crystals of 1,1-bis(4-hydroxyphenyl)-4-(trans-4-n-propylcyclohexyl)cyclohexane as a diol compound of the present invention (436 g). M.P.: 222.0°-222.8° C.

Aufarbeitung

  1. stirringfurther agitating the mixture for 30 minutes
  2. additionafter completion of the dropwise addition
  3. temperatureheating the mixture
  4. temperaturecooling
  5. filtrationfiltering off crystals
  6. washwashing the crystals with water
  7. dry with materialwith toluene, drying the crystals
  8. customrecrystallizing from tetrahydrofuran solvent

Quellen und Nachweise

ORD-Eintrag
ord-e28bd19730d147eda8d50ce302c07b73
Quelldatensatz
uspto-grants-1992_10
Patentnummer
US05152918

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