HCID 23697682, compound → HCID 86700503, compound

HRID 2201340Notes

Reaction equation

HRID 2201340 reaction equation
[Br-].[CH3:2][CH:3]1[CH2:7][CH2:6][N+:5]2([CH2:11][CH2:10][CH2:9][CH2:8]2)[CH2:4]1.[F:12][S:13]([N-:16][S:17]([F:20])(=[O:19])=[O:18])(=[O:15])=[O:14].[K+]>O>[F:12][S:13]([N-:16][S:17]([F:20])(=[O:19])=[O:18])(=[O:15])=[O:14].[CH3:2][CH:3]1[CH2:7][CH2:6][N+:5]2([CH2:11][CH2:10][CH2:9][CH2:8]2)[CH2:4]1

Participants

4

Reactant 2

HCID 23697682HCID 23697682, compoundHCID 86700504HCID 86700504, compound

Product 1

HCID 86700503HCID 86700503, compoundYield 88.9%

Reagents, catalysts & solvents 1

HCID 962WaterSolvent

Procedure

In a 300 ml conical flask, 2-methyl-5-azoniaspiro[4,4]nonanebromide (50.0 g, 0.225 mol), potassium bis(fluorosulfonyl)amide (54.0 g, 0.248 mol), and 30 ml of water were added. This liquid was mixed and stirred in the air at room temperature, so that a two-layer mixture of an aqueous layer and an objective liquid was obtained. An object was extracted from the aqueous layer of the mixture with methylene chloride. The extracting solution and the liquid obtained in the stirring were combined, washed with pure water 6 times, and dried with magnesium sulfate. The mixture was gravity filtered, and the obtained filtrate was concentrated to give a liquid. The liquid was dried under reduced pressure at 60° C. for 8 hours to obtain 2-methyl-5-azoniaspiro[4,4]nonane bis(fluorosulfonyl)amide (64.11 g, 0.20 mol).

Workup

  1. additionThis liquid was mixed
  2. customan objective liquid was obtained
  3. extractionAn object was extracted from the aqueous layer of the mixture with methylene chloride
  4. customThe extracting solution and the liquid obtained in the stirring
  5. washwashed with pure water 6 times
  6. dry with materialdried with magnesium sulfate
  7. filtrationfiltered
  8. concentrationthe obtained filtrate was concentrated
  9. customto give a liquid
  10. customThe liquid was dried under reduced pressure at 60° C. for 8 hours

Sources & evidence

ORD record
ord-c336f1fe9eeb4dff92673c29a6f6cf62
Source dataset
uspto-grants-2016_06
Patent number
US09362564B2

Reaction notes

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