Dimethylformamide → Ammonium Hydroxide

HRID 1811534Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1811534
[Cl:1][C:2]1[C:7](C(O)=[O:9])=[C:6]([F:11])[C:5]([CH3:12])=[CH:4][CH:3]=1.C(Cl)Cl.C(Cl)(=O)C(Cl)=O.C[N:23]([CH:25]=[O:26])C>>[OH-:9].[NH4+:23].[Cl:1][C:2]1[C:7]([C:25]([NH2:23])=[O:26])=[C:6]([F:11])[C:5]([CH3:12])=[CH:4][CH:3]=1

Komponenten

6

Edukt 4

HCID 6228DimethylformamideHCID 6344DichloromethaneHCID 65578Oxalyl chlorideHCID 27736696-Chloro-2-fluoro-3-methylbenzoic acid

Produkt 2

HCID 14923Ammonium HydroxideAusbeute 36 %HCID 27736646-Chloro-2-fluoro-3-methylbenzamide

Versuchsvorschrift

To 6-chloro-2-fluoro-3-methylbenzoic acid (10 g, 53 mmol) is added CH2Cl2 (60 mL), DMF (0.5 mL) and oxalyl chloride (9.25 mL, 106 mmol). The reaction mixture is allowed to stir until it reaches homogeneity and is then concentrated in vacuo. The residue is poured onto a 50:50 mixture of ice: 36% ammonium hydroxide to yield 6-chloro-2-fluoro-3-methylbenzamide.

Aufarbeitung

  1. concentrationis then concentrated in vacuo
  2. additionThe residue is poured onto a 50:50 mixture of ice

Quellen und Nachweise

ORD-Eintrag
ord-36a79107114642328e54f2ecccfbd40d
Quelldatensatz
uspto-grants-2013_01
Patentnummer
US08362294B2

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