Hydrochloric Acid → HCID 86663294, Verbindung

HRID 2364918Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 2364918
[CH3:1][C:2]1[CH:3]=[C:4]([OH:10])[CH:5]=[CH:6][C:7]=1[N:8]=[O:9].C1N2CN3CN(C2)CN1C3.Cl.FC(F)(F)[C:24](O)=[O:25]>>[OH:10][C:4]1[CH:3]=[C:2]([CH3:1])[C:7]([N:8]=[O:9])=[CH:6][C:5]=1[CH:24]=[O:25]

Komponenten

5

Versuchsvorschrift

In a 500 mL recovery flask, 5.0 g (36.5 mmol) of 3-methyl-4-nitrosophenol (manufacture by Aldrich Inc.) and 7.63 g (54.7 mmol, 1.5 eq) of hexamethylenetetramine (manufactured by Tokyo Chemical Industry Co., Ltd.) were dissolved in 100 ml of trifluoroacetic acid (manufactured by Kanto Chemical Co., Inc.) and reacted at 95° C. for 10 hours. After the reaction was completed, in an ice bath, 200 ml of 1 N hydrochloric acid was added thereto and the resultant was stirred for 15 minutes. After the stirring, the resultant was extracted with chloroform to obtain an extract. The extract was washed with hydrochloric acid and unsaturated saline, thereby obtaining 1.51 g (9.13 mmol) of 2-hydroxy-4-methyl-5-nitroso-benzaldehyde.

Aufarbeitung

  1. customreacted at 95° C. for 10 hours
  2. customAfter the reaction was completed, in an ice bath
  3. extractionAfter the stirring, the resultant was extracted with chloroform
  4. customto obtain an extract
  5. washThe extract was washed with hydrochloric acid and unsaturated saline

Quellen und Nachweise

ORD-Eintrag
ord-fa8f6d1729be43beaf7462ef68863f10
Quelldatensatz
uspto-grants-2014_04
Patentnummer
US08697332B2

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