4-(1-Pyrrolidinyl)piperidine → HCID 53628420, compound

HRID 1959080Notes

Reaction equation

HRID 1959080 reaction equation
[N:1]1([CH:6]2[CH2:11][CH2:10][NH:9][CH2:8][CH2:7]2)[CH2:5][CH2:4][CH2:3][CH2:2]1.[S:12](N)([NH2:15])(=[O:14])=[O:13]>O1CCOCC1>[N:1]1([CH:6]2[CH2:11][CH2:10][N:9]([S:12]([NH2:15])(=[O:14])=[O:13])[CH2:8][CH2:7]2)[CH2:5][CH2:4][CH2:3][CH2:2]1

Participants

4

Reactant 2

HCID 787034-(1-Pyrrolidinyl)piperidineHCID 82267Sulfamide

Product 1

HCID 53628420HCID 53628420, compound

Reagents, catalysts & solvents 1

HCID 312751,4-DioxaneSolvent

Procedure

A mixture of 4-pyrrolidin-1-ylpiperidine (0.67 g) and sulfamide (0.46 g) were heated at 115° C. in dry 1,4-dioxane (30 ml) for 16 h. The solvents were evaporated in vacuo and the residue partitioned between EtOAc (containing a little methanol) and H2O. The organic phase was collected and the aqueous layer further extracted with EtOAc (×2). The combined organic phases collected, dried (MgSO4) and the solvent evaporated. The residue was triturated with Et2O and filtered to give the subtitle product as a beige solid. Yield: 0.43 g

Workup

  1. customThe solvents were evaporated in vacuo
  2. customthe residue partitioned between EtOAc (
  3. additioncontaining a little methanol) and H2O
  4. customThe organic phase was collected
  5. extractionthe aqueous layer further extracted with EtOAc (×2)
  6. customThe combined organic phases collected
  7. dry with materialdried (MgSO4)
  8. customthe solvent evaporated
  9. customThe residue was triturated with Et2O
  10. filtrationfiltered

Sources & evidence

ORD record
ord-989c745429974f218275ac5243077a1b
Source dataset
uspto-grants-2013_04
Patent number
US08410123B2

Reaction notes

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