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 are heated under reflux overnight in 100 ml of concentrated hydrochloric acid. The mixture is concentrated, the residue is taken up in 20 ml of water, the mixture is rendered alkaline with potassium carbonate and extracted ten 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 ten times
- dry with materialthe extracts are dried over potassium carbonate
- concentrationconcentrated
- distillationthe residue is distilled
Sources & evidence
- ORD record
- ord-675a6290edcf469b92f6568d3aba1b4c
- Source dataset
- uspto-grants-1993_01
- Patent number
- US05177210
Reaction notes
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