Potassium Carbonate → 2,9-Diazatricyclo[5.3.0.0,2,5]decane

HRID 1975014Notes

Reaction equation

HRID 1975014 reaction equation
[N:1]12[CH2:10][CH2:9][CH:8]1[CH2:7][CH:6]1[CH:2]2[CH2:3][N:4](C(OCC)=O)[CH2:5]1.C(=O)([O-])[O-].[K+].[K+]>O>[N:1]12[CH2:10][CH2:9][CH:8]1[CH2:7][CH:6]1[CH:2]2[CH2:3][NH:4][CH2:5]1

Participants

4

Reactant 2

HCID 11430Potassium CarbonateHCID 54190177Ethyl 1,4-diazatricyclo [6.2.0.02,6]decane-4-carboxylate

Product 1

HCID 162289032,9-Diazatricyclo[5.3.0.0,2,5]decane

Reagents, catalysts & solvents 1

HCID 962WaterSolvent

Procedure

13.7 g (65.1 mmol) of ethyl 1,4-diazatricyclo[6.2.0.02,6 ]decane-4-carboxylate together with 42 g of Ba(OH)2 ×8H2O are refluxed overnight in 150 ml of water. Potassium carbonate is added, barium carbonate is filtered off with suction, and the filtrate is extracted ten times using 100 ml portions of chloroform. The extracts are dried over potassium carbonate and concentrated, and the residue is distilled.

Workup

  1. filtrationbarium carbonate is filtered off with suction
  2. extractionthe filtrate is extracted ten times
  3. dry with materialThe extracts are dried over potassium carbonate
  4. concentrationconcentrated
  5. distillationthe residue is distilled

Sources & evidence

ORD record
ord-52b3a3bafcc645e28824fe18c7fcb92c
Source dataset
uspto-grants-1994_02
Patent number
US05284855

Reaction notes

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