Potassium Carbonate → HCID 57042708, compound

HRID 596296Notes

Reaction equation

HRID 596296 reaction equation
Cl[C:2]1[N:7]=[CH:6][CH:5]=[CH:4][N:3]=1.[N:8]1([CH2:14][C:15]2[CH:29]=[CH:28][C:18]3[O:19][CH:20]([C:22]4[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=4)[O:21][C:17]=3[CH:16]=2)[CH2:13][CH2:12][NH:11][CH2:10][CH2:9]1.C(=O)([O-])[O-].[K+].[K+]>CN(C)C=O>[N:3]1[CH:4]=[CH:5][CH:6]=[N:7][C:2]=1[N:11]1[CH2:10][CH2:9][N:8]([CH2:14][C:15]2[CH:29]=[CH:28][C:18]3[O:19][CH:20]([C:22]4[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=4)[O:21][C:17]=3[CH:16]=2)[CH2:13][CH2:12]1

Participants

5

Reactant 3

HCID 11430Potassium CarbonateHCID 744042-ChloropyrimidineHCID 54009487HCID 54009487, compound

Product 1

HCID 57042708HCID 57042708, compoundYield 81.2%

Reagents, catalysts & solvents 1

HCID 6228DimethylformamideSolvent

Procedure

A solution of 5.7 g (0.05 mole) of 2-chloropyrimidine and 14.7 g (0.05 mole) of 5-(1-piperazinyl methyl)-2-phenyl benzo [d]-1,3-dioxole in 200 ml of dimethylformamide was refluxed for 9 hours in the presence of 13.8 g of dry potassium carbonate. The so-obtained salt was suction-filtered off and the solvent was evaporated off under reduced pressure. The crystallised residue was washed with water, and was then recrystallised from 110 ml of cyclohexane. There was obtained 15.2 g of 5-[4-(2-pyrimidinyl)-1 piperazinyl] methyl-2-phenyl benzo [d]-1,3-dioxole, cream-coloured crystals melting at (K) 106° C.

Workup

  1. filtrationThe so-obtained salt was suction-filtered off
  2. customthe solvent was evaporated off under reduced pressure
  3. washThe crystallised residue was washed with water
  4. customwas then recrystallised from 110 ml of cyclohexane

Sources & evidence

ORD record
ord-5b2bb6c3046044dca26c4d3182c8233d
Source dataset
uspto-grants-1977_03
Patent number
US04010267

Reaction notes

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