Ammonia → HCID 22329612, compound

HRID 1270296Notes

Reaction equation

HRID 1270296 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]=1

Participants

4

Reactant 3

HCID 222AmmoniaHCID 12162Benzonitrile, 4-bromo-HCID 25514Ammonium Bromide

Product 1

HCID 22329612HCID 22329612, compound

Procedure

4-Bromobenzonitrile (36.4 g, 0.2 mol), ammonium bromide (39.2 g, 0.4 mol) and ammonia gas (34.0 g, 2 mol) are heated under autogenous pressure in an autoclave for 9 h at 140–150° C. The autoclave contents are concentrated and extracted by stirring with ethanol. The residue is filtered off and again extracted 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

  1. concentrationThe autoclave contents are concentrated
  2. extractionextracted
  3. filtrationThe residue is filtered off
  4. extractionagain extracted
  5. stirringby stirring with ethanol
  6. concentrationconcentrated to about 100 ml
  7. filtrationThe precipitated solid is filtered off with suction
  8. washwashed with ethanol
  9. customdried

Sources & evidence

ORD record
ord-839331f7afd3491ab6355dcbdd3947a1
Source dataset
uspto-grants-2007_04
Patent number
US07202243B2

Reaction notes

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