Methanesulfonic Acid → HCID 178505345, compound

HRID 974425Notes

Reaction equation

HRID 974425 reaction equation
[S:1]([NH2:5])([NH2:4])(=[O:3])=[O:2].[CH3:6][S:7]([OH:10])(=[O:9])=[O:8].[Cl:11][CH2:12][CH2:13][C:14]#[N:15]>C(Cl)Cl.CC(C)=O>[CH3:6][S:7]([OH:10])(=[O:9])=[O:8].[S:1]([NH:5][C:14](=[NH:15])[CH2:13][CH2:12][Cl:11])(=[O:3])(=[O:2])[NH2:4]

Participants

6

Reactant 3

HCID 6395Methanesulfonic AcidHCID 109633-ChloropropionitrileHCID 82267Sulfamide

Product 1

HCID 178505345HCID 178505345, compoundYield 47.2%

Reagents, catalysts & solvents 2

HCID 180AcetoneSolventHCID 6344DichloromethaneSolvent

Conditions

Temperature
57.5 °C

Procedure

Sulfamide (9.6 g, 0.1 mole) was added to a solution of methanesulfonic acid anhydrous (48.0 g, 0.5 mole) in 3-chloropropionitrile (51.3 g, 0.6 mole). The suspension was heated at 55-60° C., for 18 hours. At the end of the reacting period, the mixture was diluted with methylene chloride (150 ml), and filtered. The solid, thus obtained, was suspended in acetone (50 ml), and the suspension filtered and the product dried, to yield 13.3 g of product.

Workup

  1. filtrationfiltered
  2. customThe solid, thus obtained
  3. filtrationthe suspension filtered
  4. customthe product dried

Sources & evidence

ORD record
ord-7b35f069fed64e369fefe85e2558834f
Source dataset
uspto-grants-1991_11
Patent number
US05068405

Reaction notes

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