Dimethyl Sulfate → HCID 18616026, compound

HRID 1263399Notes

Reaction equation

HRID 1263399 reaction equation
[CH3:1][C:2]1[C:3]([C:11]#[N:12])=[C:4]([SH:10])[CH:5]=[CH:6][C:7]=1[C:8]#[N:9].[OH-].[Na+].S(OC)(O[CH3:19])(=O)=O>O>[CH3:1][C:2]1[C:3]([C:11]#[N:12])=[C:4]([S:10][CH3:19])[CH:5]=[CH:6][C:7]=1[C:8]#[N:9]

Participants

5

Reactant 3

HCID 6497Dimethyl SulfateHCID 14798Sodium HydroxideHCID 18616045HCID 18616045, compound

Product 1

HCID 18616026HCID 18616026, compound

Reagents, catalysts & solvents 1

HCID 962WaterSolvent

Conditions

Temperature
25 °C

Procedure

50 g (0.29 mol) of 3-methyl-2,4-dicyanothiophenol were added to a solution of 23 g (0.58 mol) of NaOH in 400 ml of water, and 73 g (0.58 mol) of dimethyl sulfate were then added dropwise at 25-35° C. The mixture was stirred at 25° C. for 16 h, after which a solid had precipitated out, which was filtered off with suction, washed twice with water and then recrystallized from glacial acetic acid/water. Yield: 43 g (80%).

Workup

  1. additionwere then added dropwise at 25-35° C
  2. customafter which a solid had precipitated out
  3. filtrationwhich was filtered off with suction
  4. washwashed twice with water
  5. customrecrystallized from glacial acetic acid/water

Sources & evidence

ORD record
ord-b11a3db627c248289e05d0460f005f70
Source dataset
uspto-grants-2003_04
Patent number
US06541423B1

Reaction notes

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