N-Carbethoxyphthalimide → HCID 1548084, Verbindung

HRID 1531537Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1531537
Cl.[CH2:2]([O:9][C:10]1[CH:21]=[C:20]2[C:13]([NH:14][CH:15]=[C:16]2[CH2:17][CH2:18][NH2:19])=[CH:12][CH:11]=1)[C:3]1[CH:8]=[CH:7][CH:6]=[CH:5][CH:4]=1.C(N1[C:31](=[O:32])[C:30]2=[CH:33][CH:34]=[CH:35][CH:36]=[C:29]2[C:28]1=[O:37])(OCC)=O>C(N(CC)CC)C>[CH2:2]([O:9][C:10]1[CH:21]=[C:20]2[C:13](=[CH:12][CH:11]=1)[NH:14][CH:15]=[C:16]2[CH2:17][CH2:18][N:19]1[C:31](=[O:32])[C:30]2[C:29](=[CH:36][CH:35]=[CH:34][CH:33]=2)[C:28]1=[O:37])[C:3]1[CH:4]=[CH:5][CH:6]=[CH:7][CH:8]=1

Komponenten

4

Edukt 2

HCID 31187N-CarbethoxyphthalimideHCID 28287855-Benzyloxytryptamine hydrochloride

Produkt 1

HCID 1548084HCID 1548084, VerbindungAusbeute 99,3 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 8471TriethylamineLösungsmittel

Versuchsvorschrift

To a stirred suspension of 5-benzyloxytryptamine hydrochloride (1.0 g in 10 mL of dry tetrahydrofuran) was added triethylamine (0.50 mL) followed by N-carbethoxyphthalimide (750 mg) and the mixture heated to reflux on an oil bath. After 48 hours the reaction was cooled to room temperature, filtered and the filtrate concentrated in vacuo. The resulting solid was suspended in a mixture of hexane/methylene chloride (2.5:1, 50 mL) and filtered to give the title compound (1.3 g).

Aufarbeitung

  1. temperaturethe mixture heated
  2. temperatureto reflux on an oil bath
  3. filtrationfiltered
  4. concentrationthe filtrate concentrated in vacuo
  5. additionThe resulting solid was suspended in a mixture of hexane/methylene chloride (2.5:1, 50 mL)
  6. filtrationfiltered

Quellen und Nachweise

ORD-Eintrag
ord-bea80c8fdbdc48d694ab946c96ce418f
Quelldatensatz
uspto-grants-2001_03
Patentnummer
US06197975B1

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