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Sodium Hydroxide → 1-(2-Chloro-4,5-difluorobenzoyl)-3-(5-amino-2-methoxyphenyl)urea

HRID 349730
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 349730
[Cl:1][C:2]1[CH:24]=[C:23]([F:25])[C:22]([F:26])=[CH:21][C:3]=1[C:4]([NH:6][C:7]([NH:9][C:10]1[CH:15]=[C:14]([N+:16]([O-])=O)[CH:13]=[CH:12][C:11]=1[O:19][CH3:20])=[O:8])=[O:5].[OH-].[Na+]>C(OCC)(=O)C>[Cl:1][C:2]1[CH:24]=[C:23]([F:25])[C:22]([F:26])=[CH:21][C:3]=1[C:4]([NH:6][C:7]([NH:9][C:10]1[CH:15]=[C:14]([NH2:16])[CH:13]=[CH:12][C:11]=1[O:19][CH3:20])=[O:8])=[O:5]
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Komponenten

4

Edukt 2

HCID 14798Sodium HydroxideHCID 116681521-(2-Chloro4,5-difluorobenzoyl)-3-(2-methoxy-5-nitrophenyl)urea

Produkt 1

HCID 115665791-(2-Chloro-4,5-difluorobenzoyl)-3-(5-amino-2-methoxyphenyl)urea

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 8857Ethyl AcetateLösungsmittel

Versuchsvorschrift

2.2 g (5.7 mmol) of 1-(2-chloro-4,5-difluorobenzoyl)-3-(2-methoxy-5-nitrophenyl)urea were heated to the boiling temperature in 50 ml of ethyl acetate and admixed with 6.4 g (28.5 mmol) of SnCl2 monohydrate. After 1 hour, the mixture was allowed to cool to room temperature and the pH was adjusted to 8 using 2 N sodium hydroxide solution. The precipitate which formed was filtered off and washed with methanol, and the mother liquor was washed twice with H2O, dried and concentrated under reduced pressure. The resulting product (1.4 g) was reacted in step d without further purification.

Aufarbeitung

  1. customThe precipitate which formed
  2. filtrationwas filtered off
  3. washwashed with methanol
  4. washthe mother liquor was washed twice with H2O
  5. customdried
  6. concentrationconcentrated under reduced pressure
  7. customThe resulting product (1.4 g) was reacted in step d without further purification

Quellen und Nachweise

ORD-Eintrag
ord-1fb4996461a449f38ad9d49c6b43dfa6
Quelldatensatz
uspto-grants-2007_02
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US07179941B2

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