Sulfamide → HCID 43132025, compound

HRID 2388896Notes

Reaction equation

HRID 2388896 reaction equation
[CH3:1][N:2]1[CH2:7][CH2:6][CH:5]([NH:8][CH3:9])[CH2:4][CH2:3]1.[S:10](N)([NH2:13])(=[O:12])=[O:11]>O1CCOCC1>[CH3:9][N:8]([CH:5]1[CH2:6][CH2:7][N:2]([CH3:1])[CH2:3][CH2:4]1)[S:10]([NH2:13])(=[O:12])=[O:11]

Participants

4

Reactant 2

HCID 82267SulfamideHCID 5663231-Methyl-4-(methylamino)piperidine

Product 1

HCID 43132025HCID 43132025, compound

Reagents, catalysts & solvents 1

HCID 312751,4-DioxaneSolvent

Procedure

A solution of 1-methyl-4-(methylamino)piperidine (2.6 g) and sulfamide (4.0 g) in 1,4-dioxane (30 ml) was heated at 110° C. for 18 h. The reaction mixture was cooled, the solvent evaporated under reduced pressure and the residue dissolved in water. The aqueous solution was extracted with EtOAc which was washed with a small volume of saturated aqueous brine, dried (MgSO4) and the solvent evaporated under reduced pressure to give the subtitle product as a pale yellow solid. Yield: 1.5 g

Workup

  1. temperatureThe reaction mixture was cooled
  2. customthe solvent evaporated under reduced pressure
  3. dissolutionthe residue dissolved in water
  4. extractionThe aqueous solution was extracted with EtOAc which
  5. washwas washed with a small volume of saturated aqueous brine
  6. dry with materialdried (MgSO4)
  7. customthe solvent evaporated under reduced pressure

Sources & evidence

ORD record
ord-740263d4ae5844ac9ab498b1e3ad33fb
Source dataset
uspto-grants-2012_09
Patent number
US08269002B2

Reaction notes

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