Carbon Tetrachloride → HCID 15008713, compound

HRID 1087935Notes

Reaction equation

HRID 1087935 reaction equation
[Cl:1][C:2]1[CH:7]=[CH:6][N:5]=[C:4]([C:8]([CH3:10])=[CH2:9])[CH:3]=1.[Cl:11]N1C(=O)CCC1=O.C(Cl)(Cl)(Cl)Cl>CCCCCC>[Cl:1][C:2]1[CH:7]=[CH:6][N:5]=[C:4]([C:8]([CH2:10][Cl:11])=[CH2:9])[CH:3]=1

Participants

5

Reactant 3

HCID 5943Carbon TetrachlorideHCID 31398ChlorosuccinimideHCID 23437015HCID 23437015, compound

Product 1

HCID 15008713HCID 15008713, compoundYield 17.1%

Reagents, catalysts & solvents 1

HCID 8058HexaneSolvent

Procedure

A mixture of 4.3 g of 4-chloro-2-isopropenylpyridine, 3.8 g of N-chlorosuccinimide and 10 ml of carbon tetrachloride was stirred in an oil bath at 150° to 160° C. for hour. After the reaction mixture was cooled to room temperature, n-hexane was added thereto to remove the insoluble matter through filtration. After distilling off the solvent, the residue was purified by silica gel column chromatography (eluted with n-hexane-ethyl acetate 20:1) to obtain 0.90 g of the objective compound.

Workup

  1. customto remove the insoluble matter
  2. filtrationthrough filtration
  3. distillationAfter distilling off the solvent
  4. customthe residue was purified by silica gel column chromatography (eluted with n-hexane-ethyl acetate 20:1)

Sources & evidence

ORD record
ord-1c9eac62bc3f4a949ead1cc1907dc152
Source dataset
uspto-grants-1990_10
Patent number
US04960897

Reaction notes

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