Sodium Hydroxide → HCID 18378526, compound
Reaction equation
C([N:4]1[CH2:10][CH2:9][CH2:8][N:7]([CH3:11])[C:6]2[N:12]=[CH:13][CH:14]=[CH:15][C:5]1=2)(=O)C.[OH-].[Na+]>Cl>[CH3:11][N:7]1[CH2:8][CH2:9][CH2:10][NH:4][C:5]2[CH:15]=[CH:14][CH:13]=[N:12][C:6]1=2Participants
4
Reactant 2
Product 1
Reagents, catalysts & solvents 1
Procedure
A solution of 1-acetyl-5-methyl-2,3,4,5-tetrahydro-1H-pyrido[2,3-b][1,4]diazepine (1.7 g) in 6N hydrochloric acid (60 ml) was heated at 100° C. for 6 hours. After cooling, the mixture was basified with aqueous sodium hydroxide and extracted with ethyl acetate. The extracted organic layer was washed with brine and dried over sodium sulfate and concentrated in vacuo. The residue was washed with hexane to give 5-methyl-2,3,4,5-tetrahydro-1H-pyrido[2,3-b][1,4]diazepine (1.3 g).
Workup
- temperatureAfter cooling
- extractionextracted with ethyl acetate
- washThe extracted organic layer was washed with brine
- dry with materialdried over sodium sulfate
- concentrationconcentrated in vacuo
- washThe residue was washed with hexane
Sources & evidence
- ORD record
- ord-f4bd085952d848ae8b9f5ff0e20dc6a8
- Source dataset
- uspto-grants-2002_12
- Patent number
- US06495542B1
Reaction notes
Loading…