Chlorosulfonyl isocyanate → HCID 21691667, compound

HRID 653995Notes

Reaction equation

HRID 653995 reaction equation
[CH3:1][O:2][NH:3][S:4]([CH3:7])(=[O:6])=[O:5].Cl[S:9]([N:12]=[C:13]=[O:14])(=[O:11])=[O:10]>ClC1C=CC=CC=1>[CH3:7][S:4]([N:3]([O:2][CH3:1])[S:9]([N:12]=[C:13]=[O:14])(=[O:11])=[O:10])(=[O:6])=[O:5]

Participants

4

Reactant 2

HCID 70918Chlorosulfonyl isocyanateHCID 542697N-Methoxymethanesulfonamide

Product 1

HCID 21691667HCID 21691667, compound

Reagents, catalysts & solvents 1

HCID 7964ChlorobenzeneSolvent

Procedure

3.4 g (0.0272 mol) of O-methyl-N -methylsulfonylhydroxylamine (prepared in accordance with Z. Naturforsch. 36b, 1673 (1981)) are suspended in 80 ml of anhydrous chlorobenzene, and 2.53 ml (4.10 g; 0.029 mol) of chlorosulfonyl isocyanate are added at 0° C. The reaction mixture is then heated slowly while nitrogen is passed through, during which process the suspension changes into a clear solution at 40° C. After the mixture has been refluxed for about 3 hours, it is cooled and evaporated in a rotary evaporator, and the residue is dried under a high vacuum. 6.18 g (99% of theory) of N-methylsulfonyl-methoxyamino-sulfonyl isocyanate which can be employed in the next step without further purification are obtained.

Workup

  1. temperatureThe reaction mixture is then heated slowly while nitrogen
  2. customat 40° C
  3. temperatureAfter the mixture has been refluxed for about 3 hours
  4. temperatureit is cooled
  5. customevaporated in a rotary evaporator
  6. customthe residue is dried under a high vacuum
  7. custom6.18 g (99% of theory) of N-methylsulfonyl-methoxyamino-sulfonyl isocyanate which can be employed in the next step without further purification
  8. customare obtained

Sources & evidence

ORD record
ord-519d0e41a7d445d69bf3b720fc7ce04b
Source dataset
uspto-grants-1992_07
Patent number
US05129941

Reaction notes

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