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

HRID 1590140Notes

Reaction equation

HRID 1590140 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-9c0cabd6c1414062bc2282b6c139835d
Source dataset
uspto-grants-1993_04
Patent number
US05202337

Reaction notes

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