HCID 19100941, compound → 5-Chloro-2-methyl-2,7-diazabicyclo[3.3.0]octane

HRID 1975012Notes

Reaction equation

HRID 1975012 reaction equation
[Cl:1][C:2]12[CH2:9][N:8](C(OCC)=O)[CH2:7][CH:6]1[N:5]([CH3:15])[CH2:4][CH2:3]2>Cl>[Cl:1][C:2]12[CH2:9][NH:8][CH2:7][CH:6]1[N:5]([CH3:15])[CH2:4][CH2:3]2

Participants

3

Reactant 1

HCID 19100941HCID 19100941, compound

Product 1

HCID 191009765-Chloro-2-methyl-2,7-diazabicyclo[3.3.0]octane

Reagents, catalysts & solvents 1

HCID 313Hydrochloric AcidSolvent

Procedure

9.3 g (40 mmol) of ethyl 5-chloro-2-methyl-2,7-diazabicyclo[3.3. 0 ]octane-7-carboxylate are refluxed overnight together with 50 ml of concentrated hydrochloric acid. The mixture is concentrated, the concentrate is taken up in 30 ml of water, and this mixture is rendered alkaline using potassium carbonate and extracted five times using 50 ml portions of chloroform. 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-c6bfc97754184e48b85de62f7e123418
Source dataset
uspto-grants-1994_02
Patent number
US05284855

Reaction notes

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