Ethyl 2,5-dimethyl-3-oxa-2,7-diazabicyclo[3.3.0]octane-7-carboxylate → 2,5-Dimethyl-3-oxa-2,7-diazabicyclo[3.3.0]octane

HRID 345815

Reaktionsgleichung

Reaktionsgleichung von HRID 345815
[CH3:1][N:2]1[O:9][CH2:8][C:7]2([CH3:10])[CH:3]1[CH2:4][N:5](C(OCC)=O)[CH2:6]2>O>[CH3:1][N:2]1[O:9][CH2:8][C:7]2([CH3:10])[CH:3]1[CH2:4][NH:5][CH2:6]2

Komponenten

3

Edukt 1

HCID 15070010Ethyl 2,5-dimethyl-3-oxa-2,7-diazabicyclo[3.3.0]octane-7-carboxylate

Produkt 1

HCID 150700112,5-Dimethyl-3-oxa-2,7-diazabicyclo[3.3.0]octane

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 962WaterLösungsmittel

Versuchsvorschrift

13 g (60.6 mmol) of ethyl 2,5-dimethyl-3-oxa-2,7-diazabicyclo[3.3.0]octane-7-carboxylate are heated under reflux with 33 g of Ba(OH)2.8H2O in 330 ml of water overnight. The BaCO3 is filtered off with suction, K2CO3 is added to the filtrate, the solid is filtered off with suction again and the filtrate is extracted ten times with 100 ml of CHCl3 each time. The extracts are dried over K2CO3 and concentrated and the residue is distilled.

Aufarbeitung

  1. filtrationThe BaCO3 is filtered off with suction, K2CO3
  2. additionis added to the filtrate
  3. filtrationthe solid is filtered off with suction again
  4. extractionthe filtrate is extracted ten times with 100 ml of CHCl3 each time
  5. dry with materialThe extracts are dried over K2CO3
  6. concentrationconcentrated
  7. distillationthe residue is distilled

Quellen und Nachweise

ORD-Eintrag
ord-8a25500a2fdf4cf981d2acc05cfb34ce
Quelldatensatz
uspto-grants-1991_10
Patentnummer
US05059597

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