Methane → HCID 131712826, compound

HRID 1702835Notes

Reaction equation

HRID 1702835 reaction equation
[Cl:1][C:2]1[C:11]([CH3:12])=[N:10][C:9]2[C:4](=[CH:5][CH:6]=[CH:7][CH:8]=2)[N:3]=1.C.[CH3:14][NH:15][C:16]([NH:18][CH3:19])=[S:17]>CO>[ClH:1].[CH3:12][C:11]1[C:2]([S:17][C:16](=[N:15][CH3:14])[NH:18][CH3:19])=[N:3][C:4]2[C:9]([N:10]=1)=[CH:8][CH:7]=[CH:6][CH:5]=2

Participants

5

Reactant 3

HCID 297MethaneHCID 2362762-Chloro-3-methylquinoxalineHCID 2723631N,N'-Dimethylthiourea

Product 1

HCID 131712826HCID 131712826, compound

Reagents, catalysts & solvents 1

HCID 887MethanolSolvent2×

Procedure

2-Chloro-3-methylquinoxaline (3.572 g., 0.02 mole) was dissolved in 17 ml. of methanol, treated with Norit and filtered. The filtrate was added to 2.084 g. (0.02 mole) N,N'-dimethylthiourea dissolved in 25 ml. of methanol. The solution was stirred at reflux for 4 hours, cooled, and evaporated to a solid residue. The residue was triturated successively with ether and acetone, filtered and dried to give 3.554 g., 62.8% of product, m.p. 130°-131.5°.

Workup

  1. filtrationfiltered
  2. additionThe filtrate was added to 2.084 g
  3. temperatureat reflux for 4 hours
  4. temperaturecooled
  5. customevaporated to a solid residue
  6. customThe residue was triturated successively with ether and acetone
  7. filtrationfiltered
  8. customdried
  9. customto give 3.554 g

Sources & evidence

ORD record
ord-76385b5075914299a32047922fb680e1
Source dataset
uspto-grants-1982_09
Patent number
US04349674

Reaction notes

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