Dimethyl Sulfate → HCID 53675961, compound

HRID 1467828Notes

Reaction equation

HRID 1467828 reaction equation
[CH3:1][C:2]1[C:10]2[C:9](=[O:11])[N:8]([CH3:12])[C:7](=[O:13])[N:6]([CH3:14])[C:5]=2[NH:4][N:3]=1.[CH3:15]OS(OC)(=O)=O>[OH-].[Na+].O>[CH3:15][N:3]1[C:2]([CH3:1])=[C:10]2[C:5]([N:6]([CH3:14])[C:7](=[O:13])[N:8]([CH3:12])[C:9]2=[O:11])=[N:4]1

Participants

5

Reactant 2

HCID 6497Dimethyl SulfateHCID 178434199HCID 178434199, compound

Product 1

HCID 53675961HCID 53675961, compound

Reagents, catalysts & solvents 2

HCID 962WaterSolventHCID 14798Sodium HydroxideSolvent

Procedure

A solution of Step 4 intermediate (5.2 g, 26.77 mmol) in 1 N sodium hydroxide (52 ml) was added dimetylsulphate (5.2 ml) and stirred at room temperature for 1 h. The reaction mixture was diluted with water and the solid precipitated out was filtered, washed with water and dried to give 3.85 g of the product as off white solid; 1H NMR (300 MHz, CDCl3): δ 2.59 (s, 3H), 3.36 (s, 3H), 3.48 (s, 3H), 3.79 (s, 3H).

Workup

  1. customthe solid precipitated out
  2. filtrationwas filtered
  3. washwashed with water
  4. customdried

Sources & evidence

ORD record
ord-c4b9398811394b40a4a271b9001f7b7c
Source dataset
uspto-grants-2015_04
Patent number
US09000159B2

Reaction notes

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