Tris(hydroxymethyl)nitromethane → 1-benzyl-6-hydroxymethyl-4-methyl-6-nitrohexahydro-1H-1,4-diazepine

HRID 374112

Reaktionsgleichung

Reaktionsgleichung von HRID 374112
[OH:1][CH2:2][C:3]([CH2:9]O)([CH2:7]O)[N+:4]([O-:6])=[O:5].C(=O)(O)[O-].[Na+].[CH2:16]([NH:23][CH2:24][CH2:25][NH:26][CH3:27])[C:17]1[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=1>O>[CH2:16]([N:23]1[CH2:9][C:3]([CH2:2][OH:1])([N+:4]([O-:6])=[O:5])[CH2:7][N:26]([CH3:27])[CH2:25][CH2:24]1)[C:17]1[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=1

Komponenten

5

Edukt 3

HCID 31337Tris(hydroxymethyl)nitromethaneHCID 516892Sodium BicarbonateHCID 10920861N~1~-Benzyl-N~2~-methylethane-1,2-diamine

Produkt 1

HCID 149386381-benzyl-6-hydroxymethyl-4-methyl-6-nitrohexahydro-1H-1,4-diazepine

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 962WaterLösungsmittel

Reaktionsbedingungen

Temperatur
50 °C

Versuchsvorschrift

To a mixture of tris(hydroxymethyl)nitromethane (118.9 g), sodium bicarbonate (40 g) and water (1000 ml), N-benzyl-N'-methylethylenediamine (123 g) is added, and the reaction mixture is heated at about 50° C. for 2 hours. After cooling, the solution is extracted with dichloromethane, and the organic layer is washed with saturated aqueous sodium chloride and dried over magnesium sulfate. The solvent is evaporated under reduced pressure to give 1-benzyl-6-hydroxymethyl-4-methyl-6-nitrohexahydro-1H-1,4-diazepine as an oil.

Aufarbeitung

  1. additionis added
  2. temperatureAfter cooling
  3. extractionthe solution is extracted with dichloromethane
  4. washthe organic layer is washed with saturated aqueous sodium chloride
  5. dry with materialdried over magnesium sulfate
  6. customThe solvent is evaporated under reduced pressure

Quellen und Nachweise

ORD-Eintrag
ord-a9b2f3e1505e4ee9b870b600161f91c4
Quelldatensatz
uspto-grants-1992_11
Patentnummer
US05166341

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