Hydrochloric Acid → HCID 23028111, compound

HRID 1160769Notes

Reaction equation

HRID 1160769 reaction equation
[H-].[Na+].[CH2:3]([SH:5])[CH3:4].[H][H].Cl[C:9]1[CH:10]=[CH:11][C:12]2[N:13]([C:15]([S:20]([NH2:23])(=[O:22])=[O:21])=[C:16]([CH2:18][CH3:19])[N:17]=2)[N:14]=1.Cl>CN(C=O)C.O>[CH2:18]([C:16]1[N:17]=[C:12]2[CH:11]=[CH:10][C:9]([S:5][CH2:3][CH3:4])=[N:14][N:13]2[C:15]=1[S:20]([NH2:23])(=[O:22])=[O:21])[CH3:19]

Participants

8

Reactant 5

HCID 313Hydrochloric AcidHCID 6343EthanethiolHCID 24758Sodium hydrideHCID 23028090HCID 23028090, compoundHCID 178418361HCID 178418361, compound

Product 1

HCID 23028111HCID 23028111, compound

Reagents, catalysts & solvents 2

HCID 962WaterSolventHCID 6228DimethylformamideSolvent

Procedure

60% sodium hydride (0.19 g, 4.75 mmol) was suspended in DMF (5.0 ml) and ethanethiol (0.29 g, 4.6 mmol) was added thereto with stirring. After evolution of hydrogen was ceased, 6-chloro-2-ethylimidazo[1,2-b]pyridazin-3-ylsulfonamide (0.30 g, 1.15 mmol) was added thereto and stirred at 50° C. for 3 hours. After the reaction was completed, the reaction solution was poured into water (50.0 ml) and adjusted to pH 2 with dilute hydrochloric acid, and the precipitated crystals were filtered, washed with water and washed with ether, to give the title compound as pale yellow crystals. The yield was 0.19 g (57.3%).

Workup

  1. stirringstirred at 50° C. for 3 hours
  2. filtrationthe precipitated crystals were filtered
  3. washwashed with water
  4. washwashed with ether

Sources & evidence

ORD record
ord-df51ef254af2499f863a6a8b5bed7d2a
Source dataset
uspto-grants-2010_10
Patent number
US07816526B2

Reaction notes

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