Triethylamine → HCID 66953038, Verbindung

HRID 1593478Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1593478
N[C@H:2]1[CH2:7][CH2:6][N:5]([C:8]([O:10][C:11]([CH3:14])([CH3:13])[CH3:12])=[O:9])[CH2:4][C@@H:3]1[C:15]([O:17][CH3:18])=[O:16].C(N([CH2:24][CH3:25])CC)C>ClCCl>[CH2:11]([O:10][C:8]([C@H:2]1[CH2:7][CH2:6][N:5]([C:8]([O:10][C:11]([CH3:14])([CH3:13])[CH3:12])=[O:9])[CH2:4][C@H:3]1[C:15]([O:17][CH3:18])=[O:16])=[O:9])[C:25]1[CH:24]=[CH:4][CH:3]=[CH:2][CH:7]=1

Komponenten

4

Edukt 2

HCID 8471TriethylamineHCID 10934154HCID 10934154, Verbindung

Produkt 1

HCID 66953038HCID 66953038, VerbindungAusbeute 184,6 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6344DichloromethaneLösungsmittel2×

Versuchsvorschrift

A solution of 260B (0.75 g, 2.90 mmol) in dichloromethane (30 mL) at 0° C. was treated with triethylamine (0.35 g, 3.48 mmol) and N-(benzyloxycarbonyoxy)succinimide (0.72 g, 2.90 mmol). The reaction mixture was allowed to warm to room temperature and was stirred for 16 hours. The reaction mixture was diluted with dichloromethane, washed with 10% citric acid (2×50 mL), then saturated NaHCO3 (2×50 mL). The organic layer was dried over Na2SO4 and concentrated in vacuo to give 1.01 g (yield: 89%) of Compound 260C as an oil. It was used in the next step without further purification.

Aufarbeitung

  1. washwashed with 10% citric acid (2×50 mL)
  2. dry with materialThe organic layer was dried over Na2SO4
  3. concentrationconcentrated in vacuo

Quellen und Nachweise

ORD-Eintrag
ord-a5f3f3e728544f389ac552fb4e59a3bb
Quelldatensatz
uspto-grants-2007_11
Patentnummer
US07297695B2

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