Tert-Butylamine → HCID 178432181, Verbindung

HRID 1576671Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1576671
N[C:2]1C([N+]([O-])=O)=CC=C[C:3]=1OCC1OC1.C(N)(C)(C)C.[C:21]([NH:25][CH2:26][CH:27]([OH:40])[CH2:28][O:29][C:30]1[CH:35]=[CH:34][CH:33]=[C:32]([N+:36]([O-])=O)[C:31]=1[NH2:39])([CH3:24])([CH3:23])[CH3:22]>C(O)C>[CH3:2][C:3]1[NH:39][C:31]2[C:30]([O:29][CH2:28][CH:27]([OH:40])[CH2:26][NH:25][C:21]([CH3:24])([CH3:23])[CH3:22])=[CH:35][CH:34]=[CH:33][C:32]=2[N:36]=1

Komponenten

5

Edukt 3

HCID 6385Tert-ButylamineHCID 113448381-(2-Amino-3-nitrophenoxy)-2,3-epoxypropaneHCID 216815491-(2-Amino-3-nitrophenoxy)-3-(tert-butylamino)propan-2-ol

Produkt 1

HCID 178432181HCID 178432181, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 702EthanolLösungsmittel

Versuchsvorschrift

10.5 g. of the above 1-(2-amino-3-nitrophenoxy)-2,3-epoxy-propane were stirred for 30 hours at ambient temperature with 35 g. tert.-butylamine and 100 ml. ethanol. Subsequently, the reaction mixture was evaporated to dryness, the residue was dissolved in 200 ml. 2N hydrochloric acid, a small amount of undissolved material was filtered off with suction and the hydrochloric acid solution was shaken out several times with chlorofrom. 100 ml. 10N aqueous sodium hydroxide solution were then added to the aqueous acidic solution and the mixture extracted several times with ether. The ethereal extracts were dried over anhydrous sodium sulfate and then evaporated to about 100 ml., the base thereby separating out as a fine crystalline slurry by the use of ice cooling. There were obtained 10.5 g. 1-tert.-butylamino-2-hydroxy-3-(2-amino-3-nitrophenoxy)-propane; m.p. 75° - 77°C.

Aufarbeitung

  1. customSubsequently, the reaction mixture was evaporated to dryness
  2. dissolutionthe residue was dissolved in 200 ml
  3. filtration2N hydrochloric acid, a small amount of undissolved material was filtered off with suction
  4. addition10N aqueous sodium hydroxide solution were then added to the aqueous acidic solution
  5. extractionthe mixture extracted several times with ether
  6. dry with materialThe ethereal extracts were dried over anhydrous sodium sulfate
  7. customevaporated to about 100 ml
  8. custom, the base thereby separating out as a fine crystalline slurry by the use of ice cooling
  9. customThere were obtained 10.5 g

Quellen und Nachweise

ORD-Eintrag
ord-2579766efdbd48978de105de4e14a837
Quelldatensatz
uspto-grants-1976_09
Patentnummer
US03982012

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