Methyl iodide → HCID 12898280, compound

HRID 543565Notes

Reaction equation

HRID 543565 reaction equation
[CH:1]([CH:5]1[NH:10][NH:9][C:8](=[S:11])[N:7]([CH3:12])[C:6]1=[O:13])([CH2:3][CH3:4])[CH3:2].[OH-].[Na+].[CH3:16]I>O>[CH:1]([C:5]1[C:6](=[O:13])[N:7]([CH3:12])[C:8]([S:11][CH3:16])=[N:9][N:10]=1)([CH2:3][CH3:4])[CH3:2]

Participants

5

Reactant 3

HCID 6328Methyl iodideHCID 14798Sodium HydroxideHCID 13377185HCID 13377185, compound

Product 1

HCID 12898280HCID 12898280, compound

Reagents, catalysts & solvents 1

HCID 962WaterSolvent

Procedure

1 ml of 3-benzyl-4-hydroxy-biphenyl polyglycol ether, as an emulsifier, and 995 g (5 mol) of 6-sec.-butyl-4-methyl-5-oxo-3-thioxo-tetrahydro-1,2,4(2H,4H)-triazine (IX) were added to a solution of 202 g of NaOH in 5 liters of water. 724 g (5.1 mol) of methyl iodide were added dropwise and the mixture was subsequently stirred until the slightly exothermic reaction had ended and the pH value had reached 7-8. After filtering off the product, washing it with water and drying it at 30° C. in vacuo, 907 g (85% of theory) of the compound (IIb) of melting point 45°-50° C. were obtained. The crude product was sufficiently pure for further reaction. A sample recrystallised from pentane melted at 54°-55° C.

Workup

  1. filtrationAfter filtering off the product
  2. washwashing it with water
  3. customdrying it at 30° C. in vacuo, 907 g (85% of theory) of the compound (IIb) of melting point 45°-50° C.
  4. customwere obtained
  5. customA sample recrystallised from pentane melted at 54°-55° C.

Sources & evidence

ORD record
ord-6dda263fe131491ba7373cfefc2e250b
Source dataset
uspto-grants-1984_05
Patent number
US04447258

Reaction notes

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