Ammonia → HCID 45122229, compound

HRID 607191Notes

Reaction equation

HRID 607191 reaction equation
Br[C:2]1[N:9]=[C:8]([CH:10]([CH3:12])[CH3:11])[CH:7]=[CH:6][C:3]=1[C:4]#[N:5].[NH3:13]>C(O)C>[NH2:13][C:2]1[N:9]=[C:8]([CH:10]([CH3:12])[CH3:11])[CH:7]=[CH:6][C:3]=1[C:4]#[N:5]

Participants

4

Reactant 2

HCID 222AmmoniaHCID 84689561HCID 84689561, compound

Product 1

HCID 45122229HCID 45122229, compoundYield 93%

Reagents, catalysts & solvents 1

HCID 702EthanolSolvent

Procedure

To a solution of the product of Example 36C (21 g, 0.093 mol) and liquid ammonia (250 mL) in 500 mL of ethanol were reacted in a sealed high-pressure vessel at 130° C. for 20 hours. The reaction mixture was concentrated under vacuum and the residue ground to a fine powder then washed with water (2×50 mL) and dried in a vacuum oven for 24 hours to provide the title compound as a beige solid (14 g, 93%).

Workup

  1. concentrationThe reaction mixture was concentrated under vacuum
  2. washthe residue ground to a fine powder then washed with water (2×50 mL)
  3. customdried in a vacuum oven for 24 hours

Sources & evidence

ORD record
ord-47916cfefb9b49ebb75bca2e67613ca9
Source dataset
uspto-grants-2011_03
Patent number
US07915411B2

Reaction notes

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