Sodium Carbonate → 4-Amino-n-sec-butyl-n-ethyl-3-toluidine

HRID 1977539Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1977539
[CH:1]([N:5]([CH2:15][CH3:16])[C:6]1[CH:11]=[CH:10][C:9]([N:12]=O)=[C:8]([CH3:14])[CH:7]=1)([CH2:3][CH3:4])[CH3:2].C(=O)([O-])[O-].[Na+].[Na+].C1C(=NNC2C=CC(/C=C/C3C=CC(NN=C4C=CC(=O)C=C4)=CC=3S([O-])(=O)=O)=C(S([O-])(=O)=O)C=2)C=CC(=O)C=1.[Na+].[Na+]>CO.Cl.[Fe]>[NH2:12][C:9]1[CH:10]=[CH:11][C:6]([N:5]([CH:1]([CH2:3][CH3:4])[CH3:2])[CH2:15][CH3:16])=[CH:7][C:8]=1[CH3:14]

Komponenten

7

Edukt 3

HCID 10340Sodium CarbonateHCID 21993243n-Sec-butyl-n-ethyl-4-nitroso-3-toluidineHCID 178516258HCID 178516258, Verbindung

Produkt 1

HCID 219932414-Amino-n-sec-butyl-n-ethyl-3-toluidine

Reagenzien, Katalysatoren, Lösungsmittel 3

HCID 23925IronKatalysator2×HCID 313Hydrochloric AcidLösungsmittelHCID 887MethanolLösungsmittel2×

Versuchsvorschrift

A suspension of iron powder (8.34 g) in methanol (60 ml) and hydrochloric acid (20 ml) was stirred at reflux for 15 mins. A solution of the product from Stage 1d (11 g) in methanol (60 ml) was added dropwise over 15 mins and refluxing continued for 3 hours. Sodium carbonate was added until no soluble iron remained and the solution was alkaline to Brilliant Yellow paper. The hot reaction mixture was filtered and the solvent removed under reduced pressure to give the product as a brown oil.

Aufarbeitung

  1. temperatureat reflux for 15 mins
  2. temperaturerefluxing
  3. filtrationThe hot reaction mixture was filtered
  4. customthe solvent removed under reduced pressure

Quellen und Nachweise

ORD-Eintrag
ord-07c4917aba174374bbdaf7185009b95a
Quelldatensatz
uspto-grants-2001_05
Patentnummer
US06235096B1

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