Water → HCID 13784093, compound

HRID 569980Notes

Reaction equation

HRID 569980 reaction equation
[CH2:1]([N:8]1[CH2:13][CH2:12][N:11]([C:14]2[N:19]=[C:18]([CH3:20])[C:17]([C:21]([O:23]CC)=[O:22])=[CH:16][N:15]=2)[CH2:10][CH2:9]1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[OH-].[K+].O>CCO>[CH2:1]([N:8]1[CH2:13][CH2:12][N:11]([C:14]2[N:19]=[C:18]([CH3:20])[C:17]([C:21]([OH:23])=[O:22])=[CH:16][N:15]=2)[CH2:10][CH2:9]1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1

Participants

5

Reactant 3

HCID 962WaterHCID 14797Potassium HydroxideHCID 13784091HCID 13784091, compound

Product 1

HCID 13784093HCID 13784093, compoundYield 98%

Reagents, catalysts & solvents 1

HCID 702EthanolSolvent

Conditions

Temperature
100 °C

Procedure

Added to a 1 l flask were 40 g (0.128 mol) of the ethyl 2-(4-benzylpiperazino)-4-methylpyrimidine-5-carboxylate, 11 g of KOH, 200 ml of H2O and 500 ml of EtOH. The contents were stirred at 100° C. for 0.5 hr. Thereafter, the solvent was distilled off under reduced pressure. One liter of H2O was then added to the residue and the resulting mixture was adjusted to pH 4 with conc. hydrochloric acid. The precipitated crystals were filtered off and the filtrate was dried under reduced pressure, thereby obtaining 36 g of the intended compound as a white solid substance (yield: 98%).

Workup

  1. additionAdded to a 1 l flask
  2. distillationThereafter, the solvent was distilled off under reduced pressure
  3. additionOne liter of H2O was then added to the residue
  4. filtrationThe precipitated crystals were filtered off
  5. customthe filtrate was dried under reduced pressure

Sources & evidence

ORD record
ord-a82869e4cd0348bb84a77ca69efb8ef2
Source dataset
uspto-grants-1988_03
Patent number
US04734418

Reaction notes

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