Potassium Carbonate → 853297-25-3

HRID 1038727Notes

Reaction equation

HRID 1038727 reaction equation
[CH3:1][N:2]([CH2:4][C:5]1[CH:10]=[CH:9][C:8]([NH:11]C2C=C(N)N=CN=2)=[CH:7][C:6]=1[C:19]([F:22])([F:21])[F:20])[CH3:3].C([O-])([O-])=O.[K+].[K+]>CO>[CH3:3][N:2]([CH2:4][C:5]1[CH:10]=[CH:9][C:8]([NH2:11])=[CH:7][C:6]=1[C:19]([F:20])([F:22])[F:21])[CH3:1]

Participants

4

Reactant 2

HCID 11430Potassium CarbonateHCID 66669985N-(4-Dimethylaminomethyl-3-trifluoromethyl-phenyl)-pyrimidine-4,6-diamine

Product 1

HCID 57431457853297-25-3

Reagents, catalysts & solvents 1

HCID 887MethanolSolvent

Procedure

N-(4-Dimethylaminomethyl-3-trifluoromethyl-phenyl)-pyrimidine-4,6-diamine (359 mg, 1.2 mmol) is dissolved in MeOH (12 mL) and treated with K2CO3 (6 mL of a 1N aqueous solution) at RT. The reaction is heated to reflux for 1.5 h until completion, cooled back to RT and concentrated. The residual oil is taken up in EtOAc and washed with brine. The organic layers are dried over Na2SO4, filtered and concentrated under reduced pressure. Drying under high vacuum gives the title compound as a yellow oil. ESI-MS: 219 [MH]+.

Workup

  1. temperatureThe reaction is heated
  2. temperatureto reflux for 1.5 h until completion
  3. concentrationconcentrated
  4. washwashed with brine
  5. dry with materialThe organic layers are dried over Na2SO4
  6. filtrationfiltered
  7. concentrationconcentrated under reduced pressure
  8. customDrying under high vacuum

Sources & evidence

ORD record
ord-547a90d6e0bf477dbebae5d6d7812efa
Source dataset
uspto-grants-2013_10
Patent number
US08552002B2

Reaction notes

Loading…