Potassium Carbonate → HCID 14653306, compound

HRID 893312Notes

Reaction equation

HRID 893312 reaction equation
Cl[CH2:2][C:3]1[N:4]([C:17]2[CH:22]=[CH:21][CH:20]=[CH:19][C:18]=2[Cl:23])[C:5](=[O:16])[C:6]2[C:11]3[CH2:12][CH2:13][CH2:14][CH2:15][C:10]=3[S:9][C:7]=2[N:8]=1.C(=O)([O-])[O-].[K+].[K+].[CH2:30]([N:32]1[CH2:37][CH2:36][NH:35][CH2:34][CH2:33]1)[CH3:31]>C(Cl)(Cl)Cl>[Cl:23][C:18]1[CH:19]=[CH:20][CH:21]=[CH:22][C:17]=1[N:4]1[C:5](=[O:16])[C:6]2[C:11]3[CH2:12][CH2:13][CH2:14][CH2:15][C:10]=3[S:9][C:7]=2[N:8]=[C:3]1[CH2:2][N:35]1[CH2:36][CH2:37][N:32]([CH2:30][CH3:31])[CH2:33][CH2:34]1

Participants

5

Reactant 3

HCID 11430Potassium CarbonateHCID 791961-EthylpiperazineHCID 19892046HCID 19892046, compound

Product 1

HCID 14653306HCID 14653306, compoundYield 68.4%

Reagents, catalysts & solvents 1

HCID 6212ChloroformSolvent

Procedure

In 40 ml of chloroform was dissolved 820 mg of 3,4,5,6,7,8-hexahydro-2-chloromethyl-3-(2-chlorophenyl)-4-oxo(1)-benzothieno[2,3-d]pyrimidine, and 300 mg of potassium carbonate was added. Further, 310 mg of 1-ethylpiperazine was added dropwise. The mixture was heated under reflux for 5 hours. The reaction mixture was filtered, and the filtrate was concentrated under reduced pressure to give an oily substance, which was purified by silica gel chromatography. The obtained white crystals were recrystallized from ethanol to give 680 mg of the title compound, m.p. 140°-142° C.

Workup

  1. additionwas added
  2. temperatureThe mixture was heated
  3. temperatureunder reflux for 5 hours
  4. filtrationThe reaction mixture was filtered
  5. concentrationthe filtrate was concentrated under reduced pressure
  6. customto give an oily substance, which
  7. customwas purified by silica gel chromatography
  8. customThe obtained white crystals were recrystallized from ethanol

Sources & evidence

ORD record
ord-12470b37015042b7b2cfae4aab352cae
Source dataset
uspto-grants-1992_06
Patent number
US05124331

Reaction notes

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