Chloroform → HCID 17751529, compound

HRID 453338Notes

Reaction equation

HRID 453338 reaction equation
[O:1]1[CH2:7][CH:6]([CH2:8][NH2:9])[CH2:5][O:4][C:3]2[CH:10]=[CH:11][CH:12]=[CH:13][C:2]1=2.[S:14](N)([NH2:17])(=[O:16])=[O:15].C(Cl)(Cl)Cl>O1CCOCC1>[O:1]1[CH2:7][CH:6]([CH2:8][NH:9][S:14]([NH2:17])(=[O:16])=[O:15])[CH2:5][O:4][C:3]2[CH:10]=[CH:11][CH:12]=[CH:13][C:2]1=2

Participants

5

Reactant 3

HCID 6212ChloroformHCID 82267SulfamideHCID 57443657HCID 57443657, compound

Product 1

HCID 17751529HCID 17751529, compound

Reagents, catalysts & solvents 1

HCID 312751,4-DioxaneSolvent

Procedure

((3,4-Dihydro-2H-benzo[b][1,4]dioxepin-3-yl)methyl)amine (2.90 g, 16.2 mmol) and sulfamide (3.11 g, 32.4 mmol) were combined in dry dioxane (60 ml) and heated to reflux overnight. Chloroform was added and the precipitate was removed by filtration. The filtrate was concentrated under vacuum and purified by chromatography (2% to 8% acetone in dichloromethane) to yield the title compound as an off-white solid.

Workup

  1. temperatureheated
  2. temperatureto reflux overnight
  3. customthe precipitate was removed by filtration
  4. concentrationThe filtrate was concentrated under vacuum
  5. custompurified by chromatography (2% to 8% acetone in dichloromethane)

Sources & evidence

ORD record
ord-1f661de4e5574e4ea1aeca85fbf509c3
Source dataset
uspto-grants-2013_07
Patent number
US08492431B2

Reaction notes

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