Methylamine → HCID 15023185, compound

HRID 1078184Notes

Reaction equation

HRID 1078184 reaction equation
Cl[C:2]1[C:6]([C:7]2[C:12]([Cl:13])=[CH:11][CH:10]=[CH:9][C:8]=2[Cl:14])=[N:5][S:4][N:3]=1.[CH3:15][NH2:16]>O>[Cl:14][C:8]1[CH:9]=[CH:10][CH:11]=[C:12]([Cl:13])[C:7]=1[C:6]1[C:2]([NH:16][CH3:15])=[N:3][S:4][N:5]=1

Participants

4

Reactant 2

HCID 6329MethylamineHCID 10264857HCID 10264857, compound

Product 1

HCID 15023185HCID 15023185, compound

Reagents, catalysts & solvents 1

HCID 962WaterSolvent

Conditions

Temperature
120 °C

Procedure

In a stainless steel vessel, 5.31 g of 3-chloro-4-(2,6-dichlorophenyl)-1,2,5-thiadiazole and 100 ml of 40% aqueous methylamine solution were placed. After sealing the vessel, the solution was stirred at 120° C. for 12 hours. After allowing to cool, the mixture was poured into water and was extracted with ether. The ether layer was washed three times with water and three times with saturated aqueous sodium chloride solution. The resultant was then dried over anhydrous sodium sulfate and then the resultant was concentrated, followed by purification by silica gel column chromatography to obtain 2.55 g of 3-(2,6-dichlorophenyl)-4-methylamino-1,2,5-thiadiazole.

Workup

  1. temperatureto cool
  2. extractionwas extracted with ether
  3. washThe ether layer was washed three times with water and three times with saturated aqueous sodium chloride solution
  4. dry with materialThe resultant was then dried over anhydrous sodium sulfate
  5. concentrationthe resultant was concentrated
  6. customfollowed by purification by silica gel column chromatography

Sources & evidence

ORD record
ord-2d6cc707750e4acabeae022ebc41ec56
Source dataset
uspto-grants-1996_08
Patent number
US05547920

Reaction notes

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