2,6-Difluorobenzoyl chloride → HCID 9860931, Verbindung

HRID 567683

Reaktionsgleichung

Reaktionsgleichung von HRID 567683
[NH2:1][C:2]1[CH:10]=[C:9]([F:11])[C:8]([F:12])=[CH:7][C:3]=1[C:4]([OH:6])=[O:5].[F:13][C:14]1[CH:22]=[CH:21][CH:20]=[C:19]([F:23])[C:15]=1[C:16](Cl)=O.C(NC1C=CC2N=C(C3C(F)=CC=CC=3F)OC(=O)C=2C=1)(=O)C>C(N(CC)CC)C.C1(C)C=CC=CC=1>[F:13][C:14]1[CH:22]=[CH:21][CH:20]=[C:19]([F:23])[C:15]=1[C:16]1[O:5][C:4](=[O:6])[C:3]2[CH:7]=[C:8]([F:12])[C:9]([F:11])=[CH:10][C:2]=2[N:1]=1

Komponenten

5

Edukt 3

HCID 874382,6-Difluorobenzoyl chlorideHCID 7359652-Amino-4,5-difluorobenzoic acidHCID 99488136-Acetamido-(2,6-difluoro-phenyl)-benzo[d][1,3]oxazin-4-one

Produkt 1

HCID 9860931HCID 9860931, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 22504574Toluene triethylamineLösungsmittel

Versuchsvorschrift

2-Amino-4,5-difluorobenzoic acid (0.5 g), 2,6-difluorobenzoyl chloride (0.80 mL) and triethyl amine/toluene (1/1) (18 mL) were reacted as described under (10). Reaction time 1 day. Extraction between ethyl acetate (20 mL) and HCl (2N,20 mL), followed by separation of the organic toluene and precipitated with hexane. The resulting mixture was further purified on a silicagel column using dichloromethane as eluent. The isolated fraction identified as 2-(2,6-difluoro-phenyl)-6,7-difluoro-benzo[d][1,3]oxazin-4-one (0.71 g), mp. 165 C, MS m/e: 295 M+.

Aufarbeitung

  1. customReaction time 1 day
  2. extractionExtraction between ethyl acetate (20 mL) and HCl (2N,20 mL)
  3. customfollowed by separation of the organic toluene
  4. customprecipitated with hexane
  5. customThe resulting mixture was further purified on a silicagel column

Quellen und Nachweise

ORD-Eintrag
ord-a2fa7b48033c463e94febb15bcd28172
Quelldatensatz
uspto-grants-2001_01
Patentnummer
US06180625B2

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