HCID 19100966, compound → HCID 22924364, compound
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]2Participants
3
Reactant 1
Product 1
Reagents, catalysts & solvents 1
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
- concentrationThe mixture is concentrated
- extractionextracted five times
- dry with materialThe extracts are dried over potassium carbonate
- concentrationconcentrated
- distillationthe residue is distilled
Sources & evidence
- ORD record
- ord-6134c5cbd4e54b6bb0fb72d65c77b181
- Source dataset
- uspto-grants-1993_01
- Patent number
- US05177210
Reaction notes
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