HCID 19100966, compound → HCID 22924364, compound

HRID 1975011Notes

Reaction equation

HRID 1975011 reaction equation
[CH3:1][N:2]1[CH2:9][CH2:8][CH:7]2[CH:3]1[CH:4]([CH3:15])[N:5](C(OCC)=O)[CH2:6]2>Cl>[CH3:1][N:2]1[CH2:9][CH2:8][CH:7]2[CH:3]1[CH:4]([CH3:15])[NH:5][CH2:6]2

Participants

3

Procedure

16.9 g (79.6 mol) of ethyl 2,8-dimethyl-2,7-diazabicyclo[3.3.0]octane-7-carboxylate together with 130 ml of concentrated hydrochloric acid are refluxed overnight. The mixture is concentrated, the concentrate is taken up in 50 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 and concentrated, and the residue is distilled.

Workup

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

Sources & evidence

ORD record
ord-da909baf22de4a3cb2bd31d92a0406eb
Source dataset
uspto-grants-1994_02
Patent number
US05284855

Reaction notes

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