Pyridine → HCID 20455716, Verbindung

HRID 1263065

Reaktionsgleichung

Reaktionsgleichung von HRID 1263065
[Cl:1][CH:2]([CH3:10])[C:3]([NH:5][CH2:6][C:7]([OH:9])=O)=[O:4].Cl.[NH2:12][C:13]1[C:18]([OH:19])=[C:17]([Cl:20])[C:16]([CH3:21])=[C:15]([Cl:22])[CH:14]=1.N1C=CC=CC=1.S(Cl)(Cl)=O>O.C(#N)C>[Cl:1][CH:2]([CH3:10])[C:3]([NH:5][CH2:6][C:7]([NH:12][C:13]1[C:18]([OH:19])=[C:17]([Cl:20])[C:16]([CH3:21])=[C:15]([Cl:22])[CH:14]=1)=[O:9])=[O:4]

Komponenten

7

Edukt 4

HCID 1049PyridineHCID 24386Thionyl ChlorideHCID 1702236-Amino-2,4-dichloro-m-cresol hydrochlorideHCID 20455717N-(2-Chloropropanoyl)glycine

Produkt 1

HCID 20455716HCID 20455716, VerbindungAusbeute 92,2 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 962WaterLösungsmittelHCID 6342AcetonitrileLösungsmittel

Versuchsvorschrift

To a mixture composed of 158 g (0.96 mol) of N-(β-chloropropanoyl)glycine thus obtained and 92 g (0.4 mol) of 6-amino-2,4-dichloro-3-methylphenol hydrochloride were added 228 ml (2.88 mol) of pyridine and 2 liters of acetonitrile and stirred under cooling. To the solution was added dropwise 95.2 g (0.8 mol) of thionyl chloride. After the completion of the reaction, water was added to the reaction solution and the crystals thus deposited were collected by filtration and recrystallized from acetonitrile to obtain 125.2 g of 6-[α-(β-chloropropanamido)acetamido]-2,4-dichloro-3-methylphenol.

Aufarbeitung

  1. customthus obtained
  2. temperatureunder cooling
  3. additionwas added to the reaction solution
  4. filtrationthe crystals thus deposited were collected by filtration
  5. customrecrystallized from acetonitrile

Quellen und Nachweise

ORD-Eintrag
ord-5acdb209e07c4f12aa06d379c57af99f
Quelldatensatz
uspto-grants-1984_06
Patentnummer
US04455366

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