Tetrahydrofuran → HCID 23676784, compound

HRID 1492708Notes

Reaction equation

HRID 1492708 reaction equation
[H-].[Na+:2].O1CCCC1.[CH3:8][C:9]1[CH:14]=[C:13]([CH3:15])[N:12]=[C:11]([S:16]([OH:19])(=[O:18])=[O:17])[CH:10]=1>C(O)C>[CH3:8][C:9]1[CH:14]=[C:13]([CH3:15])[N:12]=[C:11]([S:16]([O-:19])(=[O:17])=[O:18])[CH:10]=1.[Na+:2]

Participants

5

Reactant 3

HCID 8028TetrahydrofuranHCID 24758Sodium hydrideHCID 15187623HCID 15187623, compound

Product 1

HCID 23676784HCID 23676784, compoundYield 100.5%

Reagents, catalysts & solvents 1

HCID 702EthanolSolvent

Procedure

In a 50 ml flask, sodium hydride (60% in oil) (200 mg, 5 mmol) and tetrahydrofuran (10 ml) were charged, and then 4,6-dimethylpyridine-2-sulfonic acid (935 mg) was gradually added at room temperature. Then, the mixture was stirred at room temperature for about 30 minutes. After the addition of a small amount of ethanol to the reaction mixture, the precipitated crystal was recovered by filtration. The crystal was washed with ethyl acetate and diethyl ether successively and dried to obtain sodium 4,6-dimethyl-2-pyridinesulfonate (1.05 g) at a quantitative yield. Melting point, 257°-258° C.

Workup

  1. filtrationthe precipitated crystal was recovered by filtration
  2. washThe crystal was washed with ethyl acetate and diethyl ether successively
  3. customdried

Sources & evidence

ORD record
ord-46b2f6d4d27b4dd2b368623753aaa1c8
Source dataset
uspto-grants-1994_12
Patent number
US05374732

Reaction notes

Loading…