Ammonia → HCID 22329612, compound
Reaction equation
[Br:1][C:2]1[CH:9]=[CH:8][C:5]([C:6]#[N:7])=[CH:4][CH:3]=1.[Br-].[NH4+:11].N>>[BrH:1].[Br:1][C:2]1[CH:9]=[CH:8][C:5]([C:6](=[NH:11])[NH2:7])=[CH:4][CH:3]=1Participants
4
Procedure
In an autoclave, 4-bromobenzonitrile (36.4 g, 200 mmol), ammonium bromide (39.2 g, 400 mmol) and ammonia gas (34.0 g, 2 mol) are heated to 140-150° C. under autogenous pressure for 9 h. The contents of the autoclave are concentrated and extracted by stirring with ethanol. The residue is filtered off and extracted again by stirring with ethanol. The extracts are combined and concentrated to about 100 ml. The precipitated solid is filtered off with suction, washed with ethanol and dried.
Workup
- concentrationThe contents of the autoclave are concentrated
- extractionextracted
- filtrationThe residue is filtered off
- extractionextracted again
- stirringby stirring with ethanol
- concentrationconcentrated to about 100 ml
- filtrationThe precipitated solid is filtered off with suction
- washwashed with ethanol
- customdried
Sources & evidence
- ORD record
- ord-5eb1dbb869b9486abd2b29e462aa4cec
- Source dataset
- uspto-grants-2005_08
- Patent number
- US06936609B2
Reaction notes
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