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Ammonium Acetate → HCID 13207875, Verbindung

HRID 918249
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 918249
[CH:1]12[CH2:7][CH:4]([CH2:5][CH2:6]1)[CH2:3][CH:2]2[CH2:8][N:9]([C:16]1[CH:29]=[CH:28][C:27]([N+:30]([O-:32])=[O:31])=[CH:26][C:17]=1[C:18]([C:20]1[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=1)=O)[C:10](=[O:15])C(Cl)(Cl)Cl.C([O-])(=O)C.[NH4+:37]>C(O)(C)(C)C>[CH:1]12[CH2:7][CH:4]([CH2:5][CH2:6]1)[CH2:3][CH:2]2[CH2:8][N:9]1[C:16]2[C:17](=[CH:26][C:27]([N+:30]([O-:32])=[O:31])=[CH:28][CH:29]=2)[C:18]([C:20]2[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=2)=[N:37][C:10]1=[O:15]
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Komponenten

4

Edukt 2

HCID 517165Ammonium Acetate2×HCID 54358427HCID 54358427, Verbindung

Produkt 1

HCID 13207875HCID 13207875, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6386tert-ButanolLösungsmittel

Versuchsvorschrift

To a solution of 2.5 g of 2-[ N-(2-norbornylmethyl)trichloroacetamido]-5-nitrobenzophenone in 50 ml of tert-butyl alcohol was added 2 g of ammonium acetate and the resulting mixture was heated under reflux for 7 hours. Then 2 g of ammonium acetate was added thereto and the reaction was continued for additional 8 hours. The solvent was removed under reduced pressure, and the residue was extracted with chloroform. The chloroform extract was washed with water, dried over anhydrous sodium sulfate, and evaporated to dryness. The residual oil was crystallized from a mixture of carbon tetrachloride and diethyl ether to give 1-(2-norbornylmethyl)-4-phenyl-6-nitro-2(1H)-quinazolinone, m.p. 160°C.

Aufarbeitung

  1. temperaturethe resulting mixture was heated
  2. temperatureunder reflux for 7 hours
  3. customThe solvent was removed under reduced pressure
  4. extractionthe residue was extracted with chloroform
  5. extractionThe chloroform extract
  6. washwas washed with water
  7. dry with materialdried over anhydrous sodium sulfate
  8. customevaporated to dryness
  9. customThe residual oil was crystallized from a mixture of carbon tetrachloride and diethyl ether

Quellen und Nachweise

ORD-Eintrag
ord-8f1e1147a88e41e3ae2d089d948350a5
Quelldatensatz
uspto-grants-1976_07
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US03970654

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