Dimethylformamide → Ammonium Hydroxide

HRID 2044195Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 2044195
[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-6dc6942cca3b4cc0b730150c345d5ce0
Quelldatensatz
uspto-grants-2013_11
Patentnummer
US08586782B2

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