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Hydrochloric Acid → 3-((1-Ethylpropyl)amino)-6-methyl-2,4-dinitrobenzyl alcohol

HRID 1388080
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1388080
C([O:4][CH2:5][C:6]1[C:11]([CH3:12])=[CH:10][C:9]([N+:13]([O-:15])=[O:14])=[C:8]([NH:16][CH:17]([CH2:20][CH3:21])[CH2:18][CH3:19])[C:7]=1[N+:22]([O-:24])=[O:23])(=O)C.Cl.O>CO>[CH2:18]([CH:17]([NH:16][C:8]1[C:7]([N+:22]([O-:24])=[O:23])=[C:6]([C:11]([CH3:12])=[CH:10][C:9]=1[N+:13]([O-:15])=[O:14])[CH2:5][OH:4])[CH2:20][CH3:21])[CH3:19]
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Komponenten

5

Edukt 3

HCID 313Hydrochloric AcidHCID 962WaterHCID 129407633-[(1-Ethylpropyl)amino]-6-methyl-2,4-dinitrobenzyl acetate

Produkt 1

HCID 1566883-((1-Ethylpropyl)amino)-6-methyl-2,4-dinitrobenzyl alcohol

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 887MethanolLösungsmittel

Versuchsvorschrift

A sample of 3-[(1-ethylpropyl)amino]-6-methyl-2,4-dinitrobenzyl acetate (23.1 g; 0.068 mol) is added to a mixture of concentrated hydrochloric acid (30 ml), water (40 ml) and methanol (320 ml). The reaction mixture is refluxed for 4 hours, cooled down and concentrated in vacuo. It is then diluted with water, extracted with ether, and the ether layer dried. The ether is removed in vacuo to leave a red oil, which readily solidifies to a yellow-orange solid (19.9 g; 98.5%). A similarly prepared and purified sample has a melting point of 51°-54° C.

Aufarbeitung

  1. temperatureThe reaction mixture is refluxed for 4 hours
  2. temperaturecooled down
  3. concentrationconcentrated in vacuo
  4. additionIt is then diluted with water
  5. extractionextracted with ether
  6. dry with materialthe ether layer dried
  7. customThe ether is removed in vacuo
  8. customto leave a red oil, which
  9. customA similarly prepared
  10. custompurified sample

Quellen und Nachweise

ORD-Eintrag
ord-a511479cec494c52a2a9ecfcc5e3981b
Quelldatensatz
uspto-grants-1984_02
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US04430114

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