Potassium Carbonate → HCID 22341120, compound

HRID 584683Notes

Reaction equation

HRID 584683 reaction equation
Cl[C:2]1[C:11]([CH2:12][CH2:13][CH2:14]Cl)=[N:10][C:9]2[C:4](=[CH:5][C:6]([Cl:17])=[C:7]([Cl:16])[CH:8]=2)[N:3]=1.[SH-:18].[Na+].C(=O)([O-])[O-].[K+].[K+]>CN(C=O)C>[Cl:16][C:7]1[CH:8]=[C:9]2[C:4](=[CH:5][C:6]=1[Cl:17])[N:3]=[C:2]1[C:11]([CH2:12][CH2:13][CH2:14][S:18]1)=[N:10]2

Participants

5

Reactant 3

HCID 11430Potassium CarbonateHCID 28015Sodium hydrosulfideHCID 22341136HCID 22341136, compound

Product 1

HCID 22341120HCID 22341120, compoundYield 100%

Reagents, catalysts & solvents 1

HCID 6228DimethylformamideSolvent

Procedure

To a solution of 2,6,7-trichloro-3-(3-chloropropyl)quinoxaline (0.15 g, 0.48 mmol) in dry DMF (50 ml) were added sodium hydrosulfide (0.11 g, 1.44 mmol) and potassium carbonate (0.20 g, 1.45 mmol). The reaction mixture was stirred for 4 days at room temperature. The solvent was evaporated in vacuo, followed by the addition of water. The resulting mixture was extracted with dichloromethane (3×). The combined organic layers were dried over anhydrous sodium sulfate, filtered and evaporated in vacuo to yield 6,7-dichloro-3,4-dihydro-2H-1-thia-9,10-diaza-anthracene (>100%) as a solid.

Workup

  1. customThe solvent was evaporated in vacuo
  2. additionfollowed by the addition of water
  3. extractionThe resulting mixture was extracted with dichloromethane (3×)
  4. dry with materialThe combined organic layers were dried over anhydrous sodium sulfate
  5. filtrationfiltered
  6. customevaporated in vacuo

Sources & evidence

ORD record
ord-d5b5f3b0e424436f94b7bfabd800e215
Source dataset
uspto-grants-2005_08
Patent number
US06927214B1

Reaction notes

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