Methylamine → 4-Nitro-(2-methylaminoethoxy)benzene

HRID 322631

Reaktionsgleichung

Reaktionsgleichung von HRID 322631
[N+:1]([C:4]1[CH:9]=[CH:8][C:7]([O:10][CH2:11][CH2:12]Cl)=[CH:6][CH:5]=1)([O-:3])=[O:2].[CH3:14][NH2:15]>C(O)(C)C.[Cl-].[Na+].O>[N+:1]([C:4]1[CH:9]=[CH:8][C:7]([O:10][CH2:11][CH2:12][NH:15][CH3:14])=[CH:6][CH:5]=1)([O-:3])=[O:2]

Komponenten

5

Edukt 2

HCID 6329MethylamineHCID 27645871-(2-Chloroethoxy)-4-nitrobenzene

Produkt 1

HCID 122944674-Nitro-(2-methylaminoethoxy)benzene

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 3776IsopropanolLösungsmittelHCID 57417360Sodium chloride; waterLösungsmittel

Versuchsvorschrift

A mixture of 4-nitro-(2-chloroethoxy)benzene (781 mg, 3.9 mmol) and aqueous methylamine (15 mL, 40 wt. %) in isopropyl alcohol (15 mL) is heated in a sealed tube at 100° for 4 hours. After cooling in an ice water bath, the mixtured is poured into brine and extracted 2× with dichloromethane, dried over sodium sulfate, filtered, and concentrated in vacuo to give 4-nitro-(2-methylaminoethoxy)benzene (697 mg).

Aufarbeitung

  1. temperatureis heated in a sealed tube at 100° for 4 hours
  2. temperatureAfter cooling in an ice water bath
  3. extractionextracted 2× with dichloromethane
  4. dry with materialdried over sodium sulfate
  5. filtrationfiltered
  6. concentrationconcentrated in vacuo

Quellen und Nachweise

ORD-Eintrag
ord-ab2a837b24004feb9e81f2c4770ebd7d
Quelldatensatz
uspto-grants-2001_04
Patentnummer
US06211365B1

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