Chloroform → HCID 17751529, compound

HRID 1428639Notes

Reaction equation

HRID 1428639 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-9b61fe27c1b4494dbd1717afbf75bb35
Source dataset
uspto-grants-2015_01
Patent number
US08937096B2

Reaction notes

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