Phosgene → HCID 14533714, compound

HRID 373352Notes

Reaction equation

HRID 373352 reaction equation
Cl.[CH3:2][Si:3]([CH3:11])([CH2:8][CH2:9][NH2:10])[Si:4]([CH3:7])([CH3:6])[CH3:5].[C:12](Cl)(Cl)=[O:13]>C1(C)C=CC=CC=1>[CH3:2][Si:3]([CH3:11])([CH2:8][CH2:9][N:10]=[C:12]=[O:13])[Si:4]([CH3:7])([CH3:6])[CH3:5]

Participants

4

Reactant 2

HCID 6371PhosgeneHCID 19812443HCID 19812443, compound

Product 1

HCID 14533714HCID 14533714, compound

Reagents, catalysts & solvents 1

HCID 1140TolueneSolvent

Procedure

50 g of 2-(pentamethyldisilanyl)ethylamine hydrochloride is suspended in 100 ml of dry toluene in a 250 ml two-neck flask fitted with a gas inlet tube and reflux condenser. A powerful stream of gaseous phosgene is then passed through the solution while stirring. At the same time the solution is heated to boiling. The conversion of the hydrochloride to the isocyanate is terminated when a clear toluene solution has been produced. Subsequently, the excess toluene is distilled off in a water-jet vacuum and the residue left behind is fractionated in an oil-pump vacuum.

Workup

  1. customfitted with a gas inlet tube
  2. temperaturereflux condenser
  3. temperatureAt the same time the solution is heated to boiling
  4. customThe conversion of the hydrochloride to the isocyanate is terminated when a clear toluene solution
  5. customhas been produced
  6. distillationSubsequently, the excess toluene is distilled off in a water-jet vacuum
  7. waitthe residue left behind

Sources & evidence

ORD record
ord-00f0bb8a512c4a74bf0bc7f2cb2c70ca
Source dataset
uspto-grants-1992_11
Patent number
US05162559

Reaction notes

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