Sodium Hydroxide → HCID 22117333, compound

HRID 965008Notes

Reaction equation

HRID 965008 reaction equation
[OH-].[Na+].[OH:3][CH2:4][CH2:5][CH2:6][SH:7].Cl[C:9]1[CH:14]=[CH:13][N+:12]([O-:15])=[C:11]([CH3:16])[C:10]=1[CH3:17]>CN1CCCC1=O>[CH3:16][C:11]1[C:10]([CH3:17])=[C:9]([S:7][CH2:6][CH2:5][CH2:4][OH:3])[CH:14]=[CH:13][N+:12]=1[O-:15]

Participants

5

Reactant 3

HCID 14798Sodium HydroxideHCID 882113-MercaptopropanolHCID 98774464-Chloro-2,3-dimethyl-1-oxidopyridin-1-ium

Product 1

HCID 22117333HCID 22117333, compound

Reagents, catalysts & solvents 1

HCID 13387N-methyl-2-pyrrolidoneSolvent2×

Procedure

6 g (60% pure) of NaOH are added in portions to 50 ml of dry N-methylpyrrolidone (NMP), the mixture is stirred for 15 min, 9.5 g (0.11 mol) of 3-hydroxypropyl mercaptan are metered in over a period of 20 min. and the mixture is stirred again for 30 min. until the evolution of gas has ended. A solution of 14.4 g (0.1 mol) of 4-chloro-2,3-dimethylpyridine N-oxide in 100 ml of NMP is then added dropwise in the course of 20 min. and the reaction mixture is stirred at room temperature for 1 hour, subsequently at 70° C. for 1 hour and thereafter at 100° C. for a further hour.

Workup

  1. customare metered in over a period of 20 min.
  2. stirringthe mixture is stirred again for 30 min. until the evolution of gas
  3. stirringthe reaction mixture is stirred at room temperature for 1 hour, subsequently at 70° C. for 1 hour
  4. waitat 100° C. for a further hour

Sources & evidence

ORD record
ord-44a449d7c22144caa8039f4186573ccd
Source dataset
uspto-grants-1998_06
Patent number
US05773451

Reaction notes

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