Gamma-Butyrolactone → HCID 178520699, Verbindung

HRID 35971

Reaktionsgleichung

Reaktionsgleichung von HRID 35971
[O:1]([C@H:5]1[CH2:10][CH2:9][C@H:8]([NH2:11])[CH2:7][CH2:6]1)[N+:2]([O-:4])=[O:3].[C:12]1(=[O:17])[O:16][CH2:15][CH2:14][CH2:13]1>>[OH:17][CH2:12][CH2:13][CH2:14][C:15]([NH:11][C@H:8]1[CH2:7][CH2:6][C@H:5]([O:1][N+:2]([O-:4])=[O:3])[CH2:10][CH2:9]1)=[O:16]

Komponenten

3

Versuchsvorschrift

4.8 g (0.03 mol) trans-4-nitroxycyclohexylamine are mixed with 5.7 ml 4-butyrolactone and stirred for 3 d at room temperature. For the removal of the excess lactone, it is filtered over a silicic gel acid with ethyl acetate. After collection of the pure fractions, it is distilled in a vacuum, triturated with ether and filtered off with suction. There remain 2.1 g of the title compound of the melting point 58°-60° C., i.e. 28% of theory.

Aufarbeitung

  1. customFor the removal of the excess lactone, it
  2. filtrationis filtered over a silicic gel acid with ethyl acetate
  3. customAfter collection of the pure fractions, it
  4. distillationis distilled in a vacuum
  5. customtriturated with ether
  6. filtrationfiltered off with suction

Quellen und Nachweise

ORD-Eintrag
ord-804ea5da64ca4972b7c3a4735b112a1e
Quelldatensatz
uspto-grants-1995_05
Patentnummer
US05411989

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