Potassium Carbonate → 2,4-Dimethyl-3-oxa-2,7-diazabicyclo[3.3.0]octane

HRID 36698Notes

Reaction equation

HRID 36698 reaction equation
[CH3:1][N:2]1[O:9][CH:8]([CH3:10])[CH:7]2[CH:3]1[CH2:4][N:5](C(OCC)=O)[CH2:6]2.C([O-])([O-])=O.[K+].[K+]>O>[CH3:1][N:2]1[O:9][CH:8]([CH3:10])[CH:7]2[CH:3]1[CH2:4][NH:5][CH2:6]2

Participants

4

Reactant 2

HCID 11430Potassium CarbonateHCID 15070019Ethyl 2,4-dimethyl-3-oxa-2,7-diazabicyclo[3.3.0]octane-7-carboxylate

Product 1

HCID 150700202,4-Dimethyl-3-oxa-2,7-diazabicyclo[3.3.0]octane

Reagents, catalysts & solvents 1

HCID 962WaterSolvent

Procedure

13.2 g (61.6 mmol) of ethyl 2,4-dimethyl-3-oxa-2,7-diazabicyclo[3.3.0]octane-7-carboxylate are heated under reflux with 39 g of Ba(OH)2.8HaO in 200 ml of water overnight. K2CO3 is added, the BaCO3 is filtered off with suction and the filtrate is extracted several times with CHCl3. The extract is dried over K2CO3 and concentrated and the residue is distilled.

Workup

  1. customovernight
  2. filtrationthe BaCO3 is filtered off with suction
  3. extractionthe filtrate is extracted several times with CHCl3
  4. dry with materialThe extract is dried over K2CO3
  5. concentrationconcentrated
  6. distillationthe residue is distilled

Sources & evidence

ORD record
ord-6453d20f725444d8bac4c1eff6f36ad4
Source dataset
uspto-grants-1995_05
Patent number
US05416096

Reaction notes

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