Sodium Iodide → HCID 15631611, compound

HRID 2352333Notes

Reaction equation

HRID 2352333 reaction equation
[O:1]1[CH:5]=[CH:4][CH:3]=[C:2]1[C:6]([N:8]1[CH2:13][CH2:12][N:11]([CH2:14][CH2:15]Cl)[CH2:10][CH2:9]1)=[O:7].[I-].[Na+].[CH3:19][NH2:20]>CO>[CH3:19][NH:20][CH2:15][CH2:14][N:11]1[CH2:12][CH2:13][N:8]([C:6]([C:2]2[O:1][CH:5]=[CH:4][CH:3]=2)=[O:7])[CH2:9][CH2:10]1

Participants

5

Reactant 3

HCID 5238Sodium IodideHCID 6329MethylamineHCID 15631610HCID 15631610, compound

Product 1

HCID 15631611HCID 15631611, compoundYield 82%

Reagents, catalysts & solvents 1

HCID 887MethanolSolvent

Procedure

A solution of 1.0 g of 1-(2-furanylcarbonyl)-4-(2-chloroethyl)piperazine and 200 mg of sodium iodide in 40 ml of methanol which contained 25% of methylamine was reacted at 70° C. in a sealed tube for 24 hours. After allowing the reaction mixture to cool down, the reaction mixture was concentrated under reduced pressure and the residue was purified by column chromatography on silica gel (eluent: a 20:1:0.1 mixture of chloroform, methanol, and methanol containing 40% methylamine) to give 800 mg of crystals (yield: 82%).

Workup

  1. customwas reacted at 70° C. in a sealed tube for 24 hours
  2. temperatureto cool down
  3. concentrationthe reaction mixture was concentrated under reduced pressure
  4. customthe residue was purified by column chromatography on silica gel (eluent
  5. additiona 20:1:0.1 mixture of chloroform, methanol, and methanol containing 40% methylamine)

Sources & evidence

ORD record
ord-e393457ccbad4525a5ae904c99829b25
Source dataset
uspto-grants-1989_10
Patent number
US04876345

Reaction notes

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