Methanol → HCID 20268283, Verbindung

HRID 1719439Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1719439
[OH:1][CH2:2][C:3]([NH:5][C:6]1[CH:11]=[CH:10][CH:9]=[CH:8][CH:7]=1)=[O:4].CO.[OH-].[Na+].[Cl:16][C:17]1[CH:24]=[CH:23][CH:22]=[CH:21][C:18]=1[CH2:19]Cl>O>[Cl:16][C:17]1[CH:24]=[CH:23][CH:22]=[CH:21][C:18]=1[CH2:19][O:1][CH2:2][C:3]([NH:5][C:6]1[CH:11]=[CH:10][CH:9]=[CH:8][CH:7]=1)=[O:4]

Komponenten

6

Edukt 4

HCID 887MethanolHCID 119062-Chlorobenzyl chlorideHCID 14798Sodium HydroxideHCID 2642602-Hydroxy-N-phenylacetamide

Produkt 1

HCID 20268283HCID 20268283, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 962WaterLösungsmittel2×

Versuchsvorschrift

2-Hydroxyacetanilide (15.1 parts) is added to methanol (60 parts). Into this mixture is further added a solution of sodium hydroxide (4.8 parts) in water (14 parts). The resulting mixture is kept at 0° to 5° C. and add dropwise 2-chlorobenzyl chloride (18.3 parts) within 30 minutes, and the reaction is continued for 2 hours at 0° to 5° C., for additional 6 hours at 30° to 40° C. and further for additional 2 hours at 65° C. After completion of the reaction, the reaction mixture is poured into cold water (250 parts) and is then filtered. The filter cake obtained is washed with water and the resulting white cake is dried at 80° C. to yield the intended product (22.3 parts) having melting point 130° to 132° C.

Aufarbeitung

  1. customis kept at 0° to 5° C.
  2. customAfter completion of the reaction
  3. filtrationis then filtered
  4. customThe filter cake obtained
  5. washis washed with water
  6. customthe resulting white cake is dried at 80° C.
  7. customto yield the intended product (22.3 parts)

Quellen und Nachweise

ORD-Eintrag
ord-3144a12e631544ef95ca2a49c68d720f
Quelldatensatz
uspto-grants-1985_09
Patentnummer
US04539577

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