Triethylamine → HCID 18995783, Verbindung

HRID 374795

Reaktionsgleichung

Reaktionsgleichung von HRID 374795
[CH3:1][O:2][C:3]1[CH:8]=[CH:7][CH:6]=[CH:5][C:4]=1[N:9]1[CH2:14][CH2:13][N:12]([CH2:15][CH2:16][CH2:17][NH2:18])[CH2:11][CH2:10]1.[O:19]1[C:23]2[CH:24]=[CH:25][CH:26]=[CH:27][C:22]=2[CH:21]=[C:20]1[C:28]([Cl:30])=[O:29].C(N(CC)CC)C>C(Cl)Cl>[ClH:30].[ClH:30].[CH3:1][O:2][C:3]1[CH:8]=[CH:7][CH:6]=[CH:5][C:4]=1[N:9]1[CH2:10][CH2:11][N:12]([CH2:15][CH2:16][CH2:17][NH:18][C:28]([C:20]2[O:19][C:23]3[CH:24]=[CH:25][CH:26]=[CH:27][C:22]=3[CH:21]=2)=[O:29])[CH2:13][CH2:14]1

Komponenten

5

Edukt 3

HCID 8471TriethylamineHCID 389492-Benzofurancarbonyl chlorideHCID 104672591-(3-Aminopropyl)-4-(2-methoxyphenyl)piperazine

Produkt 1

HCID 18995783HCID 18995783, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6344DichloromethaneLösungsmittel

Versuchsvorschrift

To a stirred solution of [4-(2-methoxyphenyl)piperazinyl]propylamine (1.0 g, 0.04 mol) in 50 mL of methylene dichloride, benzofurane-2-carboxylic acid chloride (1.01 g, 0.0056 mol) and triethylamine (1 g, 0.01 mol) were added. Stirring was continued at room temperature overnight. The methylene chloride solution was washed with water, dried over anhydrous sodium sulfate and evaporated under reduced pressure. The remaining residue was subjected to preparative HPLC using silica gel column and ethyl acetate as the eluent. The title compound was separated and converted to the dihydrochloride salt with ethanolic HCl (0.9 g), m.p. 228°-232° C.

Aufarbeitung

  1. washThe methylene chloride solution was washed with water
  2. dry with materialdried over anhydrous sodium sulfate
  3. customevaporated under reduced pressure
  4. customThe title compound was separated

Quellen und Nachweise

ORD-Eintrag
ord-5237be46d3504ae4a458eac030c49b0c
Quelldatensatz
uspto-grants-1996_01
Patentnummer
US05482940

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