Hydrochloric Acid → HCID 13936991, Verbindung

HRID 979515Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 979515
[NH2:1][C:2]([NH:4][C@H:5]([C:17]([OH:19])=O)[CH2:6][C:7]1[C:12]([N+:13]([O-:15])=[O:14])=[CH:11][CH:10]=[CH:9][C:8]=1[Cl:16])=[O:3].ClC1C=CC=C([N+]([O-])=O)C=1CCl.Cl>O>[Cl:16][C:8]1[CH:9]=[CH:10][CH:11]=[C:12]([N+:13]([O-:15])=[O:14])[C:7]=1[CH2:6][CH:5]1[NH:4][C:2](=[O:3])[NH:1][C:17]1=[O:19]

Komponenten

5

Edukt 3

HCID 313Hydrochloric AcidHCID 202004981-Chloro-2-(chloromethyl)-3-nitrobenzeneHCID 53771615HCID 53771615, Verbindung

Produkt 1

HCID 13936991HCID 13936991, VerbindungAusbeute 86,5 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 962WaterLösungsmittel

Versuchsvorschrift

A mixture of DL-N-(aminocarbonyl)-2-chloro-6-nitrophenylalanine (6.15 g, 21 mmol) prepared from 2-chloro-6-nitrobenzyl chloride according to steps 1, 2 and 3 above, concentrated hydrochloric acid (70 mL) and water (70 mL) was heated on a steam bath. After 45 minutes, the mixture was cooled, filtered and the solid washed with water and dried in air to give 5-[(2-chloro-6-nitrophenyl)methyl]-2,4imidazolidinedione (4.90 g, 85%), which was used without further purification. An analytical sample was prepared by dissolving a sample of the crude material (0.6 g) in boiling ethanol (30 mL) and adding ether to precipitate pure material (0.48 g). m.p. 210°-212° C. (dec). Spectral data were in accord with the assigned structure.

Aufarbeitung

  1. temperaturethe mixture was cooled
  2. filtrationfiltered
  3. washthe solid washed with water
  4. customdried in air

Quellen und Nachweise

ORD-Eintrag
ord-f9f93c763c754fdd8973ee40b809abc0
Quelldatensatz
uspto-grants-1987_05
Patentnummer
US04668686

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