Dichloromethane → HCID 178521126, compound

HRID 1606436Notes

Reaction equation

HRID 1606436 reaction equation
[Cl:1]CCl.[OH:4][C:5]1[C:10]([C:11]([OH:13])=O)=[CH:9][N:8]=[CH:7][CH:6]=1.S(Cl)(Cl)=O>C(N(CC)CC)C>[OH:4][C:5]1[C:10]([C:11]([Cl:1])=[O:13])=[CH:9][N:8]=[CH:7][CH:6]=1

Participants

5

Reactant 3

HCID 6344DichloromethaneHCID 24386Thionyl ChlorideHCID 178524755HCID 178524755, compound

Product 1

HCID 178521126HCID 178521126, compound

Reagents, catalysts & solvents 1

HCID 8471TriethylamineSolvent

Procedure

To 80 ml. of dichloromethane solution containing 9.8 g. of 4-hydroxynicotinic acid and 10 ml. of triethylamine was added dropwise 7 ml. of thionyl chloride with stirring under ice-cooling over a period of 20 minutes and the mixture was stirred for 2 hours at room temperature. The crystals thus formed were recovered by filtration, washed with a small amount of dichloromethane, and then dried to provide 4-hydroxynicotinoyl chloride.

Workup

  1. temperaturecooling over a period of 20 minutes
  2. customThe crystals thus formed
  3. filtrationwere recovered by filtration
  4. washwashed with a small amount of dichloromethane
  5. customdried

Sources & evidence

ORD record
ord-971823382f4f475685c2ea4f34a685bf
Source dataset
uspto-grants-1976_04
Patent number
US03953428

Reaction notes

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