HCID 19100941, compound → 5-Chloro-2-methyl-2,7-diazabicyclo[3.3.0]octane
Reaction equation
[Cl:1][C:2]12[CH2:9][N:8](C(OCC)=O)[CH2:7][CH:6]1[N:5]([CH3:15])[CH2:4][CH2:3]2>Cl>[Cl:1][C:2]12[CH2:9][NH:8][CH2:7][CH:6]1[N:5]([CH3:15])[CH2:4][CH2:3]2Participants
3
Reactant 1
Product 1
Reagents, catalysts & solvents 1
Procedure
9.3 g (40 mmol) of ethyl 5-chloro-2-methyl-2,7-diazabicyclo[3.3.0]octane-7-carboxylate are refluxed overnight together with 50 ml of concentrated hydrochloric acid. The mixture is concentrated, the concentrate is taken up in 30 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, concentrated and distilled.
Workup
- concentrationThe mixture is concentrated
- extractionextracted five times
- dry with materialThe extracts are dried over potassium carbonate
- concentrationconcentrated
- distillationdistilled
Sources & evidence
- ORD record
- ord-9c0cabd6c1414062bc2282b6c139835d
- Source dataset
- uspto-grants-1993_04
- Patent number
- US05202337
Reaction notes
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