Ethyl chloroacetate → HCID 18623221, Verbindung

HRID 278899Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 278899
[H-].[Na+].[NH2:3][CH:4]([C:7]1[CH:12]=[CH:11][C:10]([F:13])=[C:9]([F:14])[CH:8]=1)[CH2:5][OH:6].Cl[CH2:16][C:17](OCC)=[O:18]>C1COCC1>[F:14][C:9]1[CH:8]=[C:7]([CH:4]2[NH:3][C:17](=[O:18])[CH2:16][O:6][CH2:5]2)[CH:12]=[CH:11][C:10]=1[F:13]

Komponenten

5

Edukt 3

HCID 7751Ethyl chloroacetateHCID 24758Sodium hydrideHCID 220488782-Amino-2-(3,4-difluorophenyl)ethanol

Produkt 1

HCID 18623221HCID 18623221, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 8028TetrahydrofuranLösungsmittel2×

Reaktionsbedingungen

Temperatur
0 °C

Versuchsvorschrift

To a suspension of NaH (8.0 mmol, 0.19 g) in 10 mL THF at 0° C. was added a solution of 2-amino-2-(3,4-difluorophenyl)-ethanol (7.51 mmol, 1.3 g) in 20 THF dropwise via an addition funnel and after 30 min ethyl chloroacetate was added dropwise via syringe. The orange colored reaction mixture was stirred for 2 hours at 0° C. and then for 2 hours at 35° C. The solvent was removed and the 5-(3,4-difluoro-phenyl)-morpholin-3-one was isolated as a thick yellow oil (0.5 g). 1H NMR showed that the product was about 85% pure and any attempts to purify it further by column chromatography were not successful. It was used in the next reaction as described below without further purification.

Aufarbeitung

  1. waitfor 2 hours at 35° C
  2. customThe solvent was removed

Quellen und Nachweise

ORD-Eintrag
ord-d8bb694e3a254c848a822cab6ff9f87c
Quelldatensatz
uspto-grants-2002_03
Patentnummer
US06362182B1

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