Methyl iodide → HCID 23155891, compound

HRID 1714795Notes

Reaction equation

HRID 1714795 reaction equation
O1CCC[CH2:2]1.[CH3:6][N:7]1[C:16](=[O:17])[C:15]2[CH2:14][CH2:13][CH2:12][CH2:11][C:10]=2[N:9]=[C:8]1[S-:18].[K+].CI>CN(C)C=O>[CH3:6][N:7]1[C:16](=[O:17])[C:15]2[CH2:14][CH2:13][CH2:12][CH2:11][C:10]=2[N:9]=[C:8]1[S:18][CH3:2]

Participants

5

Reactant 3

HCID 6328Methyl iodideHCID 8028TetrahydrofuranHCID 23701452HCID 23701452, compound

Product 1

HCID 23155891HCID 23155891, compound

Reagents, catalysts & solvents 1

HCID 6228DimethylformamideSolvent

Procedure

To a mixture of 10 ml of tetrahydrofuran and 5 ml of dimethylformamide, 340 mg of potassium 3-methyl-4-oxo-3,4,5,6,7,8-hexahydroquinazoline-2-thiolate was added, followed by addition of 210 mg of methyl iodide and an overnight's stirring at room temperature. The solution was concentrated, to which chloroform was added, followed by washing with saturated brine and drying over anhydrous magnesium sulfate. Distilling the solvent off under reduced pressure, 310 mg (quantitative) of 3-methyl-2-methylthio-5,6,7,8-tetrahydro-3H-quinazolin-4-one was obtained.

Workup

  1. additionwas added
  2. concentrationThe solution was concentrated, to which chloroform
  3. additionwas added
  4. washby washing with saturated brine
  5. dry with materialdrying over anhydrous magnesium sulfate
  6. distillationDistilling the solvent off under reduced pressure

Sources & evidence

ORD record
ord-c954db947ff84596914c90f8b74c76de
Source dataset
uspto-grants-2010_09
Patent number
US07799775B2

Reaction notes

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