Diethylamine → N,N-dimethyl-4-(2-fluoro-5-bromobenzyloxy)butylamine

HRID 1066830Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1066830
[CH2:1]([NH:3][CH2:4]C)C.[F:6][C:7]1[CH:19]=[CH:18][C:17]([Br:20])=[CH:16][C:8]=1[CH2:9][O:10][CH2:11][CH2:12][CH2:13][CH2:14]Br>O1CCCC1.C(Cl)Cl>[CH3:1][N:3]([CH2:14][CH2:13][CH2:12][CH2:11][O:10][CH2:9][C:8]1[CH:16]=[C:17]([Br:20])[CH:18]=[CH:19][C:7]=1[F:6])[CH3:4]

Komponenten

5

Edukt 2

HCID 8021DiethylamineHCID 21196139HCID 21196139, Verbindung

Produkt 1

HCID 21196124N,N-dimethyl-4-(2-fluoro-5-bromobenzyloxy)butylamine

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 6344DichloromethaneLösungsmittelHCID 8028TetrahydrofuranLösungsmittel

Versuchsvorschrift

Diethylamine (17.6 ml, 35.3 mmol) was added to a solution of 4-(2-fluoro-5-bromobenzyloxy)butyl bromide (1.2 g, 3.53 mmol) in tetrahydrofuran (18 ml). The resulting mixture was stirred at ambient temperature for about 18 hours. The reaction mixture was diluted with methylene chloride and washed with saturated sodium bicarbonate. The aqueous fraction was back extracted with methylene chloride. The organic fractions were combined and dried over sodium sulfate. The solvents were removed in vacuo. The desired title intermediate was further purified by high performance liquid chromatography.

Aufarbeitung

  1. washwashed with saturated sodium bicarbonate
  2. extractionThe aqueous fraction was back extracted with methylene chloride
  3. dry with materialdried over sodium sulfate
  4. customThe solvents were removed in vacuo
  5. customThe desired title intermediate was further purified by high performance liquid chromatography

Quellen und Nachweise

ORD-Eintrag
ord-ffa301ccf12f48d99f0b6e2c31eb9711
Quelldatensatz
uspto-grants-2001_06
Patentnummer
US06245761B1

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