HCID 19100966, compound → HCID 22924364, compound

HRID 1460768Notes

Reaction equation

HRID 1460768 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 are heated under reflux overnight with 130 ml of concentrated hydrochloric acid. The mixture is concentrated, the residue is taken up in 50 ml of water, and the mixture is rendered alkaline with potassium carbonate and extracted five times using 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
  3. dry with materialThe extracts are dried over potassium carbonate
  4. concentrationconcentrated
  5. distillationthe residue is distilled

Sources & evidence

ORD record
ord-362fc02a663d4cb39929d592b9d61f43
Source dataset
uspto-grants-1991_12
Patent number
US05071999

Reaction notes

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