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Tetrahydrofuran → 2-Palmitoylamino-3',4'-(ethylenedioxy)acetophenone

HRID 895332
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Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 895332
Cl.[NH2:2][CH2:3][C:4]([C:6]1[CH:11]=[CH:10][CH:9]=[CH:8][CH:7]=1)=[O:5].[C:12]([O-:15])(=O)[CH3:13].[Na+].[C:17](Cl)(=[O:33])[CH2:18][CH2:19][CH2:20][CH2:21][CH2:22][CH2:23][CH2:24][CH2:25][CH2:26][CH2:27][CH2:28][CH2:29][CH2:30][CH2:31][CH3:32].[O:35]1CCCC1>>[C:17]([NH:2][CH2:3][C:4]([C:6]1[CH:11]=[CH:10][C:9]2[O:35][CH2:13][CH2:12][O:15][C:8]=2[CH:7]=1)=[O:5])(=[O:33])[CH2:18][CH2:19][CH2:20][CH2:21][CH2:22][CH2:23][CH2:24][CH2:25][CH2:26][CH2:27][CH2:28][CH2:29][CH2:30][CH2:31][CH3:32]
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

5

Edukt 4

HCID 8028Tetrahydrofuran2×HCID 8206Palmitoyl chlorideHCID 517045Sodium AcetateHCID 2723597Ethanone, 2-amino-1-phenyl-, hydrochloride (1:1)

Produkt 1

HCID 223532402-Palmitoylamino-3',4'-(ethylenedioxy)acetophenone

Versuchsvorschrift

Aminoacetophenone HCl (7.1 g, 31 mmol) and tetrahydrofuran (300 ml) were placed in a 1 liter three-neck round bottom flask with a large stir bar. Sodium acetate (50% in water, 31 ml) was added in three portions to this suspension. Palmitoyl chloride (31 ml, 10% excess, 0.036 mol) in tetrahydrofuran (25 ml) was then added dropwise over 20 min to yield a dark brown solution. This mixture was then stirred for an additional 2 h at room temperature. The resultant mixture was poured into a separatory funnel to remove the aqueous solution. Chloroform/methanol (2/1, 150 ml) was then added to the organic layer and washed with water (50 ml). The yellow aqueous layer was extracted once with chloroform (50 ml). The organic solutions were pooled and rotoevaportated until almost dry. The residue was redissolved in chloroform (100 ml) and crystallized by the addition of hexane (400 ml). The flask was then cooled to 4° C. for 2 h. The crystals were filtered and washed with cold hexane until they were almost white and then dried in a fume hood overnight. The yield of the product was 27 mmol (11.6 g).

Aufarbeitung

  1. customto yield a dark brown solution
  2. customto remove the aqueous solution
  3. additionChloroform/methanol (2/1, 150 ml) was then added to the organic layer
  4. washwashed with water (50 ml)
  5. extractionThe yellow aqueous layer was extracted once with chloroform (50 ml)
  6. customuntil almost dry
  7. dissolutionThe residue was redissolved in chloroform (100 ml)
  8. customcrystallized by the addition of hexane (400 ml)
  9. temperatureThe flask was then cooled to 4° C. for 2 h
  10. filtrationThe crystals were filtered
  11. washwashed with cold hexane until they
  12. customdried in a fume hood overnight

Quellen und Nachweise

ORD-Eintrag
ord-999160059dc84cc29593b6193ed410b2
Quelldatensatz
uspto-grants-2005_07
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US06916802B2

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