Piperazine → HCID 13307194, compound

HRID 1903303Notes

Reaction equation

HRID 1903303 reaction equation
Cl[C:2]1[N:3]=[C:4]([N:12]2[CH2:16][CH2:15][CH2:14][CH2:13]2)[C:5]2[S:11][CH2:10][CH2:9][CH2:8][C:6]=2[N:7]=1.[NH:17]1[CH2:22][CH2:21][NH:20][CH2:19][CH2:18]1>C1C=CC=CC=1>[N:17]1([C:2]2[N:3]=[C:4]([N:12]3[CH2:16][CH2:15][CH2:14][CH2:13]3)[C:5]3[S:11][CH2:10][CH2:9][CH2:8][C:6]=3[N:7]=2)[CH2:22][CH2:21][NH:20][CH2:19][CH2:18]1

Participants

4

Reactant 2

HCID 4837PiperazineHCID 13307215HCID 13307215, compound

Product 1

HCID 13307194HCID 13307194, compoundYield 61.1%

Reagents, catalysts & solvents 1

HCID 241BenzeneSolvent

Procedure

10 g of 2-chloro-4-pyrrolidino-7,8-dihydro-6H-thiopyrano[3,2-d]pyrimidine, 10 g of piperazine and 50 ml of benzene were heated at a bath temperature of 70°-80° C. for 4 hours. The solvent was then distilled off and the resulting residue was dissolved in dichloromethane. The solution was washed with water and dried. The solvent was distilled off and the resulting crystals were washed thoroughly with diethyl ether to obtain 7.3 g (61% yield) of 2-piperazino-4-pyrrolidino-7,8-dihydro-6H-thiopyrano[3,2-d]pyrimidine.

Workup

  1. distillationThe solvent was then distilled off
  2. dissolutionthe resulting residue was dissolved in dichloromethane
  3. washThe solution was washed with water
  4. customdried
  5. distillationThe solvent was distilled off
  6. washthe resulting crystals were washed thoroughly with diethyl ether

Sources & evidence

ORD record
ord-5c5d03c821884c24b7d75ebd5edbb26c
Source dataset
uspto-grants-1984_03
Patent number
US04435566

Reaction notes

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