Pyridine → HCID 20314230, compound

HRID 1282755Notes

Reaction equation

HRID 1282755 reaction equation
[C:1]1([S:7]([N:10]2[CH2:14][CH2:13][NH:12][C:11]2=[O:15])(=[O:9])=[O:8])[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[C:16](Cl)([Cl:18])=[O:17].N1C=CC=CC=1>ClCCl>[Cl:18][C:16]([N:12]1[CH2:13][CH2:14][N:10]([S:7]([C:1]2[CH:2]=[CH:3][CH:4]=[CH:5][CH:6]=2)(=[O:9])=[O:8])[C:11]1=[O:15])=[O:17]

Participants

5

Reactant 3

HCID 1049PyridineHCID 6371PhosgeneHCID 12462519HCID 12462519, compound

Product 1

HCID 20314230HCID 20314230, compound

Reagents, catalysts & solvents 1

HCID 6344DichloromethaneSolvent

Procedure

A mixture of 80 parts by weight of 1-benzenesulphonyl-2-oxo-imidazolidine, 69 parts by weight of phosgene, 31.6 parts by weight of pyridine and 350 parts by volume of dichloromethane, brought together at 0°C, was stirred overnight at room temperature and subsequently evaporated to dryness. Thereafter the material was suspended in 500 parts by volume of ice water and filtered off, the residue was taken up in 500 parts by volume of dichloromethane, the solution was dried over MgSO4, filtered and again evaporated to dryness, and the residue was recrystallized from acetone/petroleum ether.

Workup

  1. custombrought together at 0°C
  2. customsubsequently evaporated to dryness
  3. filtrationfiltered off
  4. dry with materialthe solution was dried over MgSO4
  5. filtrationfiltered
  6. customagain evaporated to dryness
  7. customthe residue was recrystallized from acetone/petroleum ether

Sources & evidence

ORD record
ord-ce7a8e7f59a742d680f009c6346fafc0
Source dataset
uspto-grants-1976_08
Patent number
US03972870

Reaction notes

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