HCID 19100947, compound → HCID 15070025, compound

HRID 1975008Notes

Reaction equation

HRID 1975008 reaction equation
[CH3:1][CH:2]1[CH2:9][CH:8]2[CH:4]([CH2:5][N:6](C(OCC)=O)[CH2:7]2)[NH:3]1>Cl>[CH3:1][CH:2]1[CH2:9][CH:8]2[CH:4]([CH2:5][NH:6][CH2:7]2)[NH:3]1

Participants

3

Procedure

17 g (85.7 mmol) of ethyl 3-methyl-2,7-diazabicyclo[ 3.3.0]octane-7-carboxylate together with 100 ml of concentrated hydrochloric acid are refluxed overnight. The mixture is concentrated, the concentrate is taken up in 50 ml of water, and the mixture is rendered alkaline using potassium carbonate and extracted ten times using 50 ml portions of chloroform. The extracts are dried over potassium carbonate and concentrated, and the residue is distilled.

Workup

  1. concentrationThe mixture is concentrated
  2. extractionextracted ten times
  3. dry with materialThe extracts are dried over potassium carbonate
  4. concentrationconcentrated
  5. distillationthe residue is distilled

Sources & evidence

ORD record
ord-6975e047fa4c4f1591536950c523741b
Source dataset
uspto-grants-1994_02
Patent number
US05284855

Reaction notes

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