Sulfamide → HCID 67051286, compound

HRID 1959060Notes

Reaction equation

HRID 1959060 reaction equation
[CH3:1][C@@H:2]1[NH:7][CH2:6][CH2:5][N:4]([C:8]([O:10][C:11]([CH3:14])([CH3:13])[CH3:12])=[O:9])[CH2:3]1.[S:15](N)([NH2:18])(=[O:17])=[O:16]>O1CCOCC1>[NH2:18][S:15]([N:7]1[CH2:6][CH2:5][N:4]([C:8]([O:10][C:11]([CH3:13])([CH3:12])[CH3:14])=[O:9])[CH2:3][C@@H:2]1[CH3:1])(=[O:17])=[O:16]

Participants

4

Reactant 2

HCID 82267SulfamideHCID 7023035(S)-1-Boc-3-methylpiperazine

Product 1

HCID 67051286HCID 67051286, compound

Reagents, catalysts & solvents 1

HCID 312751,4-DioxaneSolvent

Conditions

Temperature
110 °C

Procedure

To a solution of tert-butyl (3S)-3-methylpiperazine-1-carboxylate (0.5 g) in dioxane (40 ml) was added sulfamide (0.29 g) and the reaction was heated at 110° C. for 18 h. The reaction mixture was then partitioned between DCM (150 ml) and H2O (150 ml). The organics were separated and the aqueous layer was re-extracted with DCM (2×150 ml). Organics were combined, dried (MgSO4) and reduced in vacuo to give the subtitle compound as a pale yellow oil. Yield: 0.66 g

Workup

  1. customThe reaction mixture was then partitioned between DCM (150 ml) and H2O (150 ml)
  2. customThe organics were separated
  3. extractionthe aqueous layer was re-extracted with DCM (2×150 ml)
  4. dry with materialdried (MgSO4)

Sources & evidence

ORD record
ord-e64f8b91800a4e57aa7033b7609d3112
Source dataset
uspto-grants-2013_04
Patent number
US08410123B2

Reaction notes

Loading…