Triethylamine → HCID 19378720, compound

HRID 2210431Notes

Reaction equation

HRID 2210431 reaction equation
[SH:1][C:2]1[C:7]([N+:8]([O-:10])=[O:9])=[CH:6][C:5]([CH3:11])=[CH:4][N:3]=1.C([N:14](CC)CC)C.NOS(O)(=O)=O>ClCCl.O>[CH3:11][C:5]1[CH:6]=[C:7]([N+:8]([O-:10])=[O:9])[C:2]([S:1][NH2:14])=[N:3][CH:4]=1

Participants

6

Reactant 3

HCID 8471TriethylamineHCID 76284hydroxylamine-O-sulfonic acidHCID 178430799HCID 178430799, compound

Product 1

HCID 19378720HCID 19378720, compound

Reagents, catalysts & solvents 2

HCID 962WaterSolventHCID 6344DichloromethaneSolvent

Procedure

A solution of 12 g of 2-mercapto-5-methyl-3- nitropyridine and 28.6 g of triethylamine in 180 cm3 of dichloromethane is treated dropwise with 12 g of hydroxylamine-O-sulfonic acid dissolved in the minimum amount of water. At the end of the reaction, the solvent is removed under partial vacuum and the residue is taken up in 20 cm3 of water. The precipitate obtained is collected on a filter, washed with water and dried. It is recrystallized from a dichloromethane/petroleum jelly mixture.

Workup

  1. customAt the end of the reaction
  2. customthe solvent is removed under partial vacuum
  3. customThe precipitate obtained
  4. customis collected on a filter
  5. washwashed with water
  6. customdried
  7. customIt is recrystallized from a dichloromethane/petroleum jelly mixture

Sources & evidence

ORD record
ord-90bb0d19b82f40d6add40bb5d0398327
Source dataset
uspto-grants-1995_10
Patent number
US05459138

Reaction notes

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