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

HRID 2255703Notes

Reaction equation

HRID 2255703 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[3.3.01octane-7-carboxylate are heated under reflux overnight with 50 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 and extracted five times with 50 ml of chloroform each time. The extracts are 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 materialThe extracts are dried over potassium carbonate
  4. concentrationconcentrated
  5. distillationthe residue is distilled

Sources & evidence

ORD record
ord-77175d6a8292465fa8312aa405f564c9
Source dataset
uspto-grants-1993_08
Patent number
US05241076

Reaction notes

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