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Benzyl Bromide → Methyl 2-benzyl-3-dimethylaminopropionate

HRID 280298
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 280298
[CH3:1][N:2]([CH3:11])P(N(C)C)(N(C)C)=O.CN([CH:15]([CH3:20])[C:16]([O:18][CH3:19])=[O:17])C.[CH2:21](Br)[C:22]1[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=1>O1CCCC1>[CH2:21]([CH:15]([CH2:20][N:2]([CH3:11])[CH3:1])[C:16]([O:18][CH3:19])=[O:17])[C:22]1[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=1
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

5

Edukt 3

HCID 7498Benzyl BromideHCID 12679HexamethylphosphoramideHCID 15594675Methyl 2-(dimethylamino)propanoate

Produkt 1

HCID 13653933Methyl 2-benzyl-3-dimethylaminopropionate

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 8028TetrahydrofuranLösungsmittel3×

Versuchsvorschrift

The reaction mixture is stirred for 1/2 hour at the same temperature, a solution of 179 g of hexamethylphosphoramide in 200 ml of tetrahydrofuran is added and stirring is continued for 1/2 hour at -78°. At the same temperature a solution of 125 g of methyl N,N-dimethylaminopropionate in 200 ml of tetrahydrofuran is then added dropwise and stirring is continued for 20 minutes. A solution of 171 g of benzyl bromide in 300 ml of tetrahydrofuran is then added, again at -78°. The solution is stirred at this temperature for 2 hours and then quenched, first with 250 ml of saturated aqueous ammonium chloride and then 250 ml of saturated aqueous sodium chloride solution. To this is added 1500 ml of ether. The layers are separated and the aqueous layer is extracted with 4×200 ml of ether. The ether extract is dried over magnesium sulfate and evaporated to dryness. The resulting oil is redissolved in 300 L ml of ether, the ether solution is washed with 100 ml of water and the aqueous layer is reextracted with 3×100 ml ether. The combined ether solutions are dried over magnesium sulfate and evaporated to dryness in yield an oil which is purified by fractional distillation to yield pure methyl 2-benzyl-3-dimethylaminopropionate, b.p. 104°/0.2-0.4 mm Hg.

Aufarbeitung

  1. stirringstirring
  2. waitis continued for 1/2 hour at -78°
  3. stirringstirring
  4. waitis continued for 20 minutes
  5. stirringThe solution is stirred at this temperature for 2 hours
  6. customquenched, first with 250 ml of saturated aqueous ammonium chloride
  7. additionTo this is added 1500 ml of ether
  8. customThe layers are separated
  9. extractionthe aqueous layer is extracted with 4×200 ml of ether
  10. extractionThe ether extract
  11. dry with materialis dried over magnesium sulfate
  12. customevaporated to dryness
  13. dissolutionThe resulting oil is redissolved in 300 L ml of ether
  14. washthe ether solution is washed with 100 ml of water
  15. dry with materialThe combined ether solutions are dried over magnesium sulfate
  16. customevaporated to dryness
  17. customin yield an oil which
  18. distillationis purified by fractional distillation

Quellen und Nachweise

ORD-Eintrag
ord-2d7dd60ccf2344738490d0a22164fb85
Quelldatensatz
uspto-grants-1986_05
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US04588746

Notizen zur Reaktion

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