Boron trifluoride → 2,3-Dimethyl-6-myristoyl-hydroquinone

HRID 224467

Reaktionsgleichung

Reaktionsgleichung von HRID 224467
B(F)(F)F.[CH3:5][C:6]1[C:12]([CH3:13])=[C:11]([OH:14])[CH:10]=[CH:9][C:7]=1[OH:8].[C:15](O)(=[O:29])[CH2:16][CH2:17][CH2:18][CH2:19][CH2:20][CH2:21][CH2:22][CH2:23][CH2:24][CH2:25][CH2:26][CH2:27][CH3:28].C([O-])(=O)C.[Na+]>C1C=CC=CC=1.C(Cl)Cl>[CH3:5][C:6]1[C:12]([CH3:13])=[C:11]([OH:14])[CH:10]=[C:9]([C:15](=[O:29])[CH2:16][CH2:17][CH2:18][CH2:19][CH2:20][CH2:21][CH2:22][CH2:23][CH2:24][CH2:25][CH2:26][CH2:27][CH3:28])[C:7]=1[OH:8]

Komponenten

7

Edukt 4

HCID 6356Boron trifluorideHCID 11005Myristic AcidHCID 691002,3-DimethylhydroquinoneHCID 517045Sodium Acetate

Produkt 1

HCID 205104672,3-Dimethyl-6-myristoyl-hydroquinone

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 241BenzeneLösungsmittelHCID 6344DichloromethaneLösungsmittel

Reaktionsbedingungen

Temperatur
50 °C

Versuchsvorschrift

Boron trifluoride was introduced with vigorous refluxing (bath temperature 50° C.) into a mixture of 138 g (1 mole) of 2,3-dimethylhydroquinone, 370 g (1.62 moles) of myristic acid and 700 ml of methylene chloride until saturation. After standing overnight the reaction mixture was decomposed by pouring into 3 l of a 10% by weight sodium acetate solution with stirring. The methylene chloride was evaporated by means of steam. The residual oily layer solidified after cooling to a melt cake that was isolated by decantation. It was melted up and added with stirring to 2 l of high-boiling benzine. The precipitate was filtered with suction and washed with benzine (boiling range: 50°-75° C.). After being dried the precipitate was stirred with acetonitrile and filtered with suction.

Aufarbeitung

  1. customThe methylene chloride was evaporated by means of steam
  2. temperatureafter cooling to a melt cake that
  3. customwas isolated by decantation
  4. additionadded
  5. filtrationThe precipitate was filtered with suction
  6. washwashed with benzine (boiling range: 50°-75° C.)
  7. customAfter being dried the precipitate
  8. stirringwas stirred with acetonitrile
  9. filtrationfiltered with suction

Quellen und Nachweise

ORD-Eintrag
ord-07d8b452c2364852bfe5eaac08c6343c
Quelldatensatz
uspto-grants-1980_11
Patentnummer
US04232107

Verknüpfte Notizen

Wird geladen…