HCID 19100959, compound → 5-Chloro-2,3-dimethyl-2,7-diazabicyclo[3.3.0]octane

HRID 1460774Notes

Reaction equation

HRID 1460774 reaction equation
[Cl:1][C:2]12[CH2:9][N:8](C(OCC)=O)[CH2:7][CH:6]1[N:5]([CH3:15])[CH:4]([CH3:16])[CH2:3]2>Cl>[Cl:1][C:2]12[CH2:9][NH:8][CH2:7][CH:6]1[N:5]([CH3:15])[CH:4]([CH3:16])[CH2:3]2

Participants

3

Reactant 1

HCID 19100959HCID 19100959, compound

Product 1

HCID 191009535-Chloro-2,3-dimethyl-2,7-diazabicyclo[3.3.0]octane

Reagents, catalysts & solvents 1

HCID 313Hydrochloric AcidSolvent

Procedure

7.6 g (30.8 mmol) of ethyl 5-chloro-2,3-dimethyl -2,7-diazabicyclo[3.3.0]octane-7-carboxylate are heated under reflux overnight with 30 ml of concentrated hydrochloric acid. The mixture is concentrated, the residue is taken up in 30 ml of water, and the mixture is rendered alkaline with potassium carbonate, extracted five times with 50 ml of chloroform each time, dried over potassium carbonate and concentrated, and the residue is distilled.

Workup

  1. concentrationThe mixture is concentrated
  2. extractionextracted five times with 50 ml of chloroform each time
  3. dry with materialdried over potassium carbonate
  4. concentrationconcentrated
  5. distillationthe residue is distilled

Sources & evidence

ORD record
ord-d7d525b1bf1644beb95e52e2b90c38a9
Source dataset
uspto-grants-1991_12
Patent number
US05071999

Reaction notes

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