Water → HCID 13784173, compound

HRID 570008Notes

Reaction equation

HRID 570008 reaction equation
[CH2:1]([N:8]1[CH2:13][CH2:12][N:11]([C:14]2[N:19]=[C:18]([NH:20][CH2:21][CH3:22])[C:17]([C:23]([O:25]CC)=[O:24])=[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>C(O)C>[CH2:1]([N:8]1[CH2:9][CH2:10][N:11]([C:14]2[N:19]=[C:18]([NH:20][CH2:21][CH3:22])[C:17]([C:23]([OH:25])=[O:24])=[CH:16][N:15]=2)[CH2:12][CH2:13]1)[C:2]1[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=1

Participants

5

Reactant 3

HCID 962WaterHCID 14797Potassium HydroxideHCID 13784169HCID 13784169, compound

Product 1

HCID 13784173HCID 13784173, compoundYield 82%

Reagents, catalysts & solvents 1

HCID 702EthanolSolvent2×

Procedure

After refluxing for 1 hour a mixture of 106.4 g (0.29 mol) of ethyl 2-(4-benzylpiperazino)-4-ethylaminopyrimidine-5-carboxylate (the compound synthesized in Referential Example 64), 38.0 g (0.58 mol) of a 85% aqueous solution of potassium hydroxide, 100 ml of water and 400 ml of ethanol, ethanol was distilled off under reduced pressure. The residue was added with water and then neutralized with hydrochloric acid. The precipitated crystals were collected by filtration and were then dried to obtain 80.3 g of the above-identified compound (yield: 82%).

Workup

  1. temperatureAfter refluxing for 1 hour
  2. distillationwas distilled off under reduced pressure
  3. additionThe residue was added with water
  4. filtrationThe precipitated crystals were collected by filtration
  5. customwere then dried

Sources & evidence

ORD record
ord-ae4adc93e72d44cc893b3afa1e2399d7
Source dataset
uspto-grants-1988_03
Patent number
US04734418

Reaction notes

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