HCID 19100940, compound → HCID 19100965, compound

HRID 1975034Notes

Reaction equation

HRID 1975034 reaction equation
[Br: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>[Br: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 19100940HCID 19100940, compound

Product 1

HCID 19100965HCID 19100965, compound

Reagents, catalysts & solvents 1

HCID 313Hydrochloric AcidSolvent

Procedure

18.4 g (60.7 mmol, 91.4%) of ethyl 5-bromo-2-methyl-2,7-diazabicyclo[3.3.0]octane-7-carboxylate are refluxed overnight together with 120 ml of concentrated hydrochloric acid. The mixture is concentrated, the concentrate is taken up in 50 ml of water, this mixture is rendered alkaline using potassium carbonate and extracted five times using 100 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-5367d3eb02d24f53ad263b2dafeb919e
Source dataset
uspto-grants-1994_02
Patent number
US05284855

Reaction notes

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