Triethylamine → HCID 90281983, Verbindung
Reaktionsgleichung
Cl[CH2:2][C:3]1[CH:8]=[CH:7][CH:6]=[CH:5][C:4]=1[CH2:9][C:10]([O:12][C:13]([CH3:16])([CH3:15])[CH3:14])=[O:11].Cl.[NH2:18][CH2:19][C:20]([O:22][C:23]([CH3:26])([CH3:25])[CH3:24])=[O:21].C(N(CC)CC)C>C(#N)C>[C:13]([O:12][C:10](=[O:11])[CH2:9][C:4]1[CH:5]=[CH:6][CH:7]=[CH:8][C:3]=1[CH2:2][NH:18][CH2:19][C:20]([O:22][C:23]([CH3:26])([CH3:25])[CH3:24])=[O:21])([CH3:16])([CH3:15])[CH3:14]Komponenten
5
Edukt 3
Produkt 1
Reagenzien, Katalysatoren, Lösungsmittel 1
Reaktionsbedingungen
- Temperatur
- 60 °C
Versuchsvorschrift
To a solution of tert-butyl [2-(chloromethyl)phenyl]acetate (2.31 g) in acetonitrile (23.1 mL) were added tert-butyl glycinate hydrochloride (2.41 g) and triethylamine (4.01 mL), followed by heating at 60° C. for 3 hours. The reaction suspension was concentrated under reduced pressure, then to the residue were added water and ethyl acetate, and the organic layer was extracted. The organic layer was dried over anhydrous magnesium sulfate and concentrated under reduced pressure. The residue was purified by silica gel column chromatography (hexane-ethyl acetate) to obtain tert-butyl N-[2-(2-tert-butoxy-2-oxoethyl)benzyl]glycinate (2.54 g).
Aufarbeitung
- concentrationThe reaction suspension was concentrated under reduced pressure
- additionto the residue were added water and ethyl acetate
- extractionthe organic layer was extracted
- dry with materialThe organic layer was dried over anhydrous magnesium sulfate
- concentrationconcentrated under reduced pressure
- customThe residue was purified by silica gel column chromatography (hexane-ethyl acetate)
Quellen und Nachweise
- ORD-Eintrag
- ord-cd91c40870c7472faade22b7f028fffc
- Quelldatensatz
- uspto-grants-2015_12
- Patentnummer
- US09199927B2
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