HCID 19100973, compound → HCID 19100943, compound
Reaction equation
[F:1][CH2:2][C:3]12[CH2:10][N:9](C(OCC)=O)[CH2:8][CH:7]1[N:6]([CH3:16])[CH2:5][CH2:4]2>Cl>[F:1][CH2:2][C:3]12[CH2:10][NH:9][CH2:8][CH:7]1[N:6]([CH3:16])[CH2:5][CH2:4]2Participants
3
Reactant 1
Product 1
Reagents, catalysts & solvents 1
Procedure
7.1 g (26 mmol) of ethyl 5-fluoromethyl-2-methyl-2,7-diazabicyclo[3.3.0]octane-7-carboxylate in 100 ml of concentrated hydrochloric acid are refluxed overnight. The mixture is concentrated, the concentrate is taken up in 20 ml of water, this mixture is rendered alkaline using potassium carbonate and extracted ten times using 50 ml portions of chloroform, and the extracts are dried over potassium carbonate, concentrated and distilled.
Workup
- concentrationThe mixture is concentrated
- extractionextracted ten times
- dry with materialthe extracts are dried over potassium carbonate
- concentrationconcentrated
- distillationdistilled
Sources & evidence
- ORD record
- ord-15f90691a1d34175a558224d4324b463
- Source dataset
- uspto-grants-1994_02
- Patent number
- US05284855
Reaction notes
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