Triethylamine → HCID 15729653, compound

HRID 704325Notes

Reaction equation

HRID 704325 reaction equation
Cl.[OH:2][C:3]1[CH:8]=[CH:7][CH:6]=[C:5]([OH:9])[N:4]=1.[CH3:10][S:11](Cl)(=[O:13])=[O:12].C(N(CC)CC)C>ClCCl>[CH3:10][S:11]([O:2][C:3]1[CH:8]=[CH:7][CH:6]=[C:5]([O:9][S:11]([CH3:10])(=[O:13])=[O:12])[N:4]=1)(=[O:13])=[O:12]

Participants

5

Reactant 3

HCID 8471TriethylamineHCID 31297Methanesulfonyl chlorideHCID 178479628HCID 178479628, compound

Product 1

HCID 15729653HCID 15729653, compound

Reagents, catalysts & solvents 1

HCID 6344DichloromethaneSolvent

Procedure

2,6-dihydroxypyridine hydrochloride (3 g) was suspended in dichloromethane (250 cm3) under an atmosphere of nitrogen at 0° C. The mixture was treated with methanesulphonyl chloride (3.5 cm3). The suspension was stirred and triethylamine (9.4 cm3) was added in aliquots over 15 minutes. The resulting mixture was stirred for 17 hours and poured onto brine. The organic layer was separated, washed twice with brine, dried over anhydrous magnesium sulphate, and the solvent evaporated under reduced pressure.

Workup

  1. stirringThe resulting mixture was stirred for 17 hours
  2. additionpoured onto brine
  3. customThe organic layer was separated
  4. washwashed twice with brine
  5. dry with materialdried over anhydrous magnesium sulphate
  6. customthe solvent evaporated under reduced pressure

Sources & evidence

ORD record
ord-e6b8950ab732416ba0ab4639b3e37ba3
Source dataset
uspto-grants-1991_01
Patent number
US04987141

Reaction notes

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