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Triethylamine → HCID 19780164, Verbindung

HRID 2081559
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Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 2081559
[Cl:1][C:2]1[CH:3]=[C:4]([C:16]([OH:18])=O)[C:5]2[O:10][C:9]([CH3:12])([CH3:11])[CH2:8][N:7]([CH2:13][CH3:14])[C:6]=2[CH:15]=1.C(N(CC)CC)C.C(Cl)(=O)C(C)(C)C.[NH2:33][CH:34]1[CH:39]2[CH2:40][CH2:41][N:36]([CH2:37][CH2:38]2)[CH2:35]1>C(OCC)(=O)C>[ClH:1].[Cl:1][C:2]1[CH:3]=[C:4]([C:16]([NH:33][CH:34]2[CH:39]3[CH2:40][CH2:41][N:36]([CH2:37][CH2:38]3)[CH2:35]2)=[O:18])[C:5]2[O:10][C:9]([CH3:11])([CH3:12])[CH2:8][N:7]([CH2:13][CH3:14])[C:6]=2[CH:15]=1
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

6

Edukt 4

HCID 8471TriethylamineHCID 62493Pivaloyl chlorideHCID 1232383-AminoquinuclidineHCID 19780125HCID 19780125, Verbindung

Produkt 1

HCID 19780164HCID 19780164, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 8857Ethyl Acetate
Lösungsmittel

Versuchsvorschrift

To a solution of 1.5 g of 6-chloro-2,2-dimethyl-4-ethyl-3,4-dihydro-2H-1,4-benzoxazine-8-carboxylic acid in 30 ml of ethyl acetate was added 1.56 ml of triethylamine, and 0.67 g of pivaloyl chloride was added dropwise thereto at -10° to -5° C. under cooling. After stirring for 15 minutes at the same temperature, 0.70 g of 3-aminoquinuclidine was added at -10° to -5° C. and the mixture was stirred at room temperature for an hour. The resultant mixture was washed with water, dried over magnesium sulfate and concentrated. To the residue was added ethanolic hydrochloric acid and the precipitated crystals were collected by filtration and recrystallized from ethanol to give 6-chloro-2,2-dimethyl-4-ethyl-N-(3-quinuclidinyl)-3,4-dihydro-2H-1,4-benzoxazine-8-carboxamide hydrochloride as white crystals, melting at 273°-276° C.

Aufarbeitung

  1. additionwas added dropwise
  2. temperatureat -10° to -5° C. under cooling
  3. additionwas added at -10° to -5° C.
  4. washThe resultant mixture was washed with water
  5. dry with materialdried over magnesium sulfate
  6. concentrationconcentrated
  7. additionTo the residue was added ethanolic hydrochloric acid
  8. filtrationthe precipitated crystals were collected by filtration
  9. customrecrystallized from ethanol

Quellen und Nachweise

ORD-Eintrag
ord-022d02a8b9ac428780c00c7edd85c602
Quelldatensatz
uspto-grants-1993_02
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US05185333

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