Benzyl Alcohol → 2-{[(Benzyloxy)carbonyl]amino}ethyl 2-methylprop-2-enoate

HRID 3077

Reaktionsgleichung

Reaktionsgleichung von HRID 3077
[C:1]([O:6][CH2:7][CH2:8][N:9]=[C:10]=[O:11])(=[O:5])[C:2]([CH3:4])=[CH2:3].[CH2:12]([OH:19])[C:13]1[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=1>O1CCOCC1.C([O-])(=O)CCCCCCCCCCC.C([O-])(=O)CCCCCCCCCCC.C([Sn+2]CCCC)CCC>[C:1]([O:6][CH2:7][CH2:8][NH:9][C:10]([O:19][CH2:12][C:13]1[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=1)=[O:11])(=[O:5])[C:2]([CH3:4])=[CH2:3]

Komponenten

5

Edukt 2

HCID 244Benzyl AlcoholHCID 354092-Isocyanatoethyl methacrylate

Produkt 1

HCID 138396362-{[(Benzyloxy)carbonyl]amino}ethyl 2-methylprop-2-enoateAusbeute 80,6 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 9809426Di-n-butyldilauryltinKatalysatorHCID 312751,4-DioxaneLösungsmittel

Versuchsvorschrift

77.5 g of methacryloyloxyethyl isocyanate (Karenzu MOI, available from Showa Denko K.K.) and 60 g of benzyl alcohol were dissolved in 260 g of dioxane. To the solution were then added 5 drops of di-n-butyltin dilaurate. The reaction mixture was then allowed to undergo reaction at a temperature of 65° C. for 3 hours. The dioxane and excess benzyl alcohol were then distilled off under reduced pressure. The residue was poured into water, extracted with ethyl acetate, and then dried. The solvent was then distilled off to obtain 106 g of benzyloxycarbonylaminoethyl methacrylate in the form of colorless oil.

Aufarbeitung

  1. customreaction at a temperature of 65° C. for 3 hours
  2. distillationThe dioxane and excess benzyl alcohol were then distilled off under reduced pressure
  3. additionThe residue was poured into water
  4. extractionextracted with ethyl acetate
  5. customdried
  6. distillationThe solvent was then distilled off

Quellen und Nachweise

ORD-Eintrag
ord-921b325d103d4c73b989008641f1fd3d
Quelldatensatz
uspto-grants-1998_03
Patentnummer
US05733707

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