Ammonia → HCID 178501028, compound

HRID 2391737Notes

Reaction equation

HRID 2391737 reaction equation
Cl.Cl.[NH:3]1[C:11]2[CH2:10][C@@H:9]([C:12]([O:14][CH3:15])=[O:13])[NH:8][CH2:7][C:6]=2[N:5]=[CH:4]1.N.CO>ClCCl>[NH:3]1[C:11]2[CH2:10][C@@H:9]([C:12]([O:14][CH3:15])=[O:13])[NH:8][CH2:7][C:6]=2[N:5]=[CH:4]1

Participants

5

Reactant 3

HCID 222AmmoniaHCID 887MethanolHCID 178501029HCID 178501029, compound

Product 1

HCID 178501028HCID 178501028, compoundYield 95.7%

Reagents, catalysts & solvents 1

HCID 6344DichloromethaneSolvent

Procedure

Into a mixture of 188.25 g methyl (65)-4,5,6,7-tetrahydro-imidazo[4,5-c]pyridine-6-carboxylate dihydrochloride in 3 l dichloromethane at 10-15° C. is lead gaseous ammonia until saturation takes place (about one hour). 200 ml methanol are added and the mixture is filtered. The filter cake is washed with 2×100 ml DCM/MeOH (8/2 v/v). The filtrate is concentrated under reduced pressure and the resulting solid is dried under vacuum to give 128.4 g of the title product.

Workup

  1. customplace (about one hour)
  2. filtrationthe mixture is filtered
  3. washThe filter cake is washed with 2×100 ml DCM/MeOH (8/2 v/v)
  4. concentrationThe filtrate is concentrated under reduced pressure
  5. customthe resulting solid is dried under vacuum

Sources & evidence

ORD record
ord-dd86a1f0dfc44962ae48d5e8aeee343e
Source dataset
uspto-grants-2012_09
Patent number
US08273890B2

Reaction notes

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