Sulfamide → HCID 68603983, compound

HRID 2245209Notes

Reaction equation

HRID 2245209 reaction equation
[CH2:1]([N:8]1[CH2:13][CH2:12][N:11]([CH2:14][C:15]2[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=2)[CH2:10][CH:9]1[CH2:21][NH2:22])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[S:23](N)([NH2:26])(=[O:25])=[O:24]>O1CCOCC1>[CH2:1]([N:8]1[CH2:13][CH2:12][N:11]([CH2:14][C:15]2[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=2)[CH2:10][CH:9]1[CH2:21][NH:22][S:23]([NH2:26])(=[O:25])=[O:24])[C:2]1[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=1

Participants

4

Reactant 2

HCID 82267SulfamideHCID 10085886HCID 10085886, compound

Product 1

HCID 68603983HCID 68603983, compound

Reagents, catalysts & solvents 1

HCID 312751,4-DioxaneSolvent

Conditions

Temperature
95 °C

Procedure

To a solution of 1,4-dibenzyl-2-aminomethyl-piperazine (2.5 g, 8.46 mmol) in dioxane (50 mL), was added sulfamide (1.63 g, 16.9 mmol) and the resulting mixture was stirred at 95° C. under N2 atmosphere for several hours (monitored by TLC). The solvent was removed under reduced pressure and the crude material was purified by flash chromatography on silica gel using acetonitrile/water with gradient as eluent.

Workup

  1. customThe solvent was removed under reduced pressure
  2. customthe crude material was purified by flash chromatography on silica gel

Sources & evidence

ORD record
ord-06cabfb7190c45508321df50e403f3c7
Source dataset
uspto-grants-2010_03
Patent number
US07683049B2

Reaction notes

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