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

HRID 1590141Notes

Reaction equation

HRID 1590141 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 together with 30 ml of concentrated hydrochloric acid are refluxed overnight. The mixture is concentrated, the concentrate is taken up in 30 ml of water, this mixture is rendered alkaline using potassium carbonate and extracted five times using 50 ml portions of chloroform, and the extracts are dried over potassium carbonate, concentrated and distilled.

Workup

  1. concentrationThe mixture is concentrated
  2. extractionextracted five times
  3. dry with materialthe extracts are dried over potassium carbonate
  4. concentrationconcentrated
  5. distillationdistilled

Sources & evidence

ORD record
ord-d240346758624e2d8ec55f8e8f4a3a77
Source dataset
uspto-grants-1993_04
Patent number
US05202337

Reaction notes

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