HCID 20443323, compound → HCID 13339627, compound

HRID 1632125Notes

Reaction equation

HRID 1632125 reaction equation
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([C:8](Cl)([CH3:14])[CH2:9][C:10]([Cl:13])([Cl:12])[Cl:11])=[CH:4][N:3]=1>ClC1C=CC=CC=1>[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([C:8](=[CH2:14])[CH2:9][C:10]([Cl:11])([Cl:12])[Cl:13])=[CH:4][N:3]=1

Participants

3

Reactant 1

HCID 20443323HCID 20443323, compound

Product 1

HCID 13339627HCID 13339627, compound

Reagents, catalysts & solvents 1

HCID 7964ChlorobenzeneSolvent

Procedure

A solution of 40 g (0.013 mole) of 2-chloro-5-(1,3,3,3-tetrachloro-1-methylpropyl)pyridine and 7.8 g (0.026 mole) of SbCl5 in 300 ml of chlorobenzene was heated to 138° C. for one hour. The darkened solution was cooled and carefully quenched with water. The heterogeneous mixture was filtered, the organic layer separated, dried (MgSO4) and concentrated in vacuo. The product was crystallized from 350 ml of pentane at -50° C. The yield was 19.5 g (55%), m.p. 54°-55° C.

Workup

  1. temperatureThe darkened solution was cooled
  2. customcarefully quenched with water
  3. filtrationThe heterogeneous mixture was filtered
  4. customthe organic layer separated
  5. dry with materialdried (MgSO4)
  6. concentrationconcentrated in vacuo
  7. customThe product was crystallized from 350 ml of pentane at -50° C

Sources & evidence

ORD record
ord-a88307e22e754980ad758a1f25be0477
Source dataset
uspto-grants-1984_10
Patent number
US04474602

Reaction notes

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