Water → HCID 20036192, Verbindung

HRID 1388228

Reaktionsgleichung

Reaktionsgleichung von HRID 1388228
[NH2:1][C:2]1[CH:7]=[C:6]([Cl:8])[C:5]([N+:9]([O-])=O)=[CH:4][C:3]=1[OH:12].[C:13]([C:18]1[CH:30]=[C:29]([C:31]([CH2:34][CH3:35])([CH3:33])[CH3:32])[CH:28]=[CH:27][C:19]=1[O:20][CH:21]([CH2:25][CH3:26])[C:22](Cl)=[O:23])([CH2:16][CH3:17])([CH3:15])[CH3:14].[Cl-].[NH4+].O>C(#N)C.C(O)(C)C>[NH2:9][C:5]1[C:6]([Cl:8])=[CH:7][C:2]([NH:1][C:22](=[O:23])[CH:21]([O:20][C:19]2[CH:27]=[CH:28][C:29]([C:31]([CH2:34][CH3:35])([CH3:33])[CH3:32])=[CH:30][C:18]=2[C:13]([CH2:16][CH3:17])([CH3:15])[CH3:14])[CH2:25][CH3:26])=[C:3]([OH:12])[CH:4]=1

Komponenten

7

Edukt 4

HCID 962WaterHCID 25517Ammonium ChlorideHCID 1703932-(2,4-Bis(1,1-dimethylpropyl)phenoxy)butyryl chlorideHCID 38948482-Amino-4-chloro-5-nitrophenol

Produkt 1

HCID 20036192HCID 20036192, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 3776IsopropanolLösungsmittelHCID 6342AcetonitrileLösungsmittel

Versuchsvorschrift

20 g of 2-amino-4-chloro-5-nitrophenol was dispersed in 150 ml of acetonitrile to which 37.7 g of 2-(2,4-di-tert-amylphenoxy)butanoyl chloride was added dropwise under refluxing. After refluxing for 4 hours, the reaction mixture was cooled to deposit crystals. The crystals were collected by filtration, washed with acetonitrile and dried to yield 49.5 g thereof. 49 g of the crystals were refluxed with stirring for 1 hour together with 28 g of reduced iron powder, 2.7 g of ammonium chloride, 50 ml of water and 500 ml of isopropanol. After removing the iron powder by filtration, the filtrate was cooled to deposite the crystals. The crystals were collected by filtration and dried to obtain 42.4 g of the above described compound.

Aufarbeitung

  1. additionwas added dropwise
  2. temperatureunder refluxing
  3. temperatureAfter refluxing for 4 hours
  4. temperaturethe reaction mixture was cooled
  5. filtrationThe crystals were collected by filtration
  6. washwashed with acetonitrile
  7. customdried
  8. customto yield 49.5 g
  9. customAfter removing the iron powder
  10. filtrationby filtration
  11. temperaturethe filtrate was cooled
  12. filtrationThe crystals were collected by filtration
  13. customdried
  14. customto obtain 42.4 g of the

Quellen und Nachweise

ORD-Eintrag
ord-8919f825e6f14be88bc6054fdfc71b2c
Quelldatensatz
uspto-grants-1984_02
Patentnummer
US04430423

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