Dimethylamine → HCID 174802, Verbindung

HRID 917982Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 917982
[CH3:1][C:2]1[O:3][C:4]2[CH:15]=[CH:14][C:13]([OH:16])=[C:12]([Cl:17])[C:5]=2[C:6]=1[C:7]([O:9][CH2:10][CH3:11])=[O:8].[CH3:18][NH:19][CH3:20].[CH2:21]=O>CN(C)C=O>[CH3:1][C:2]1[O:3][C:4]2[CH:15]=[C:14]([CH2:18][N:19]([CH3:21])[CH3:20])[C:13]([OH:16])=[C:12]([Cl:17])[C:5]=2[C:6]=1[C:7]([O:9][CH2:10][CH3:11])=[O:8]

Komponenten

5

Edukt 3

HCID 674DimethylamineHCID 712FormaldehydeHCID 122247863-Benzofurancarboxylic acid, 4-chloro-5-hydroxy-2-methyl-, ethyl ester

Produkt 1

HCID 174802HCID 174802, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6228DimethylformamideLösungsmittel

Versuchsvorschrift

A solution of 1.9 g of 2-methyl-3-carbethoxy-4-chloro-5-hydroxybenzofuran, 2.6 ml of a 33 percent aqueous solution of dimethylamine and 0.6 ml of 36 percent Formalin in 12 ml of dimethylformamide is refluxed at a temperature of 100° to 105° for 8 hours and then cooled to ambient temperature. The precipitated crystals are filtered off, washed with water and dried in order to yield 0.75 g of crystalline 2-methyl-3-carbethoxy-4-chloro-hydroxy-6-dimethylaminomethylbenzofuran. An additional 0.4 g of crystals is obtained from the parent solution by dilution with water. The total yield is 1.15 g (50%); m.p., 130°-131°C (from alcohol). Mixed melting of the product crystals with a specimen from Example 1a gave no depression of the melting point.

Aufarbeitung

  1. filtrationThe precipitated crystals are filtered off
  2. washwashed with water
  3. customdried in order

Quellen und Nachweise

ORD-Eintrag
ord-4ba3764374f144ec926854d8cbc85848
Quelldatensatz
uspto-grants-1976_07
Patentnummer
US03968237

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