HCID 19100948, compound → HCID 19100963, compound

HRID 1975026Notes

Reaction equation

HRID 1975026 reaction equation
[CH2:1]([N:8]1[CH2:15][CH:14]([CH3:16])[CH:13]2[CH:9]1[CH2:10][N:11](C(OCC)=O)[CH2:12]2)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1>Cl>[CH2:1]([N:8]1[CH2:15][CH:14]([CH3:16])[CH:13]2[CH:9]1[CH2:10][NH:11][CH2:12]2)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1

Participants

3

Reactant 1

HCID 19100948HCID 19100948, compound

Product 1

HCID 19100963HCID 19100963, compound

Reagents, catalysts & solvents 1

HCID 313Hydrochloric AcidSolvent

Procedure

10 g (26.3 mmol) of ethyl 2-benzyl-4-methyl-2,7-diazabicyclo[3.3.0]octane-7-carboxylate are refluxed overnight together with 100 ml of concentrated hydrochloric acid. The mixture is concentrated, the concentrate is taken up in 20 ml of water, the 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-844341aabc674ed9b8680317e60ec818
Source dataset
uspto-grants-1994_02
Patent number
US05284855

Reaction notes

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