Diphosgene → HCID 19030391, compound

HRID 266663Notes

Reaction equation

HRID 266663 reaction equation
[CH2:1]([NH:3][CH:4]1[CH2:10][CH2:9][CH2:8][CH2:7][CH2:6][CH2:5]1)[CH3:2].[Cl:11][C:12]([O:15]C(Cl)=O)(Cl)Cl>C(OCC)(=O)C>[CH:4]1([N:3]([CH2:1][CH3:2])[C:12]([Cl:11])=[O:15])[CH2:10][CH2:9][CH2:8][CH2:7][CH2:6][CH2:5]1

Participants

4

Reactant 2

HCID 10426DiphosgeneHCID 13112620N-Ethylcycloheptanamine

Product 1

HCID 19030391HCID 19030391, compoundYield 56.4%

Reagents, catalysts & solvents 1

HCID 8857Ethyl AcetateSolvent

Procedure

N-ethylcycloheptylamine (21.15 g) was added with ice bath cooling to a mixture consisting of trichloromethylchloroformate (29.7 g) end ethyl acetate (300 ml). Thereafter, the temperature was gradually elevated and heated with refluxing for 6 hours. After distilling off the solvent, the obtained oil was distilled under reduced pressure to obtain N-cycloheptyl -N-ethylcarbamoyl chloride (17.20 g). b.p. 125°-128° C./4.0 mbar.

Workup

  1. temperaturecooling to a mixture
  2. temperatureheated
  3. temperaturewith refluxing for 6 hours
  4. distillationAfter distilling off the solvent
  5. distillationthe obtained oil was distilled under reduced pressure

Sources & evidence

ORD record
ord-8416a9392e9b4ae295053020ba1fc29e
Source dataset
uspto-grants-1997_07
Patent number
US05652198

Reaction notes

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