Hydrochloric Acid → HCID 13648719, compound

HRID 1494519Notes

Reaction equation

HRID 1494519 reaction equation
[C:1]([N:5]1[C:10](=[O:11])[C:9]([Br:12])=[C:8](Br)[CH:7]=[N:6]1)([CH3:4])([CH3:3])[CH3:2].[SH-:14].[Na+].Cl>O>[C:1]([N:5]1[C:10](=[O:11])[C:9]([Br:12])=[C:8]([SH:14])[CH:7]=[N:6]1)([CH3:4])([CH3:3])[CH3:2]

Participants

5

Reactant 3

HCID 313Hydrochloric AcidHCID 28015Sodium hydrosulfideHCID 13852600HCID 13852600, compound

Product 1

HCID 13648719HCID 13648719, compoundYield 30.4%

Reagents, catalysts & solvents 1

HCID 962WaterSolvent

Conditions

Temperature
60 °C

Procedure

To 200 ml of water were added 31.0 g of 2-tert.-butyl-4,5-dibromo-3(2H)-pyridazinone and 15.8 g of 70% sodium hydrosulfide. After stirring at 60° C. for 4 hours, the resulting mixture was allowed to cool to room temperature and incorporated with about 8 ml of concentrated hydrochloric acid to lower the pH of the liquid to not higher than 2. The resulting solid was filtered off, washed with water, dried and then recrystallized from benzene/n-hexane to give 8.0g of the intended product as white crystals of m.p. 107°-110° C. (yield: 30.4%).

Workup

  1. filtrationThe resulting solid was filtered off
  2. washwashed with water
  3. customdried
  4. customrecrystallized from benzene/n-hexane

Sources & evidence

ORD record
ord-ffeaf06958db4c45bc77795c2be77d6a
Source dataset
uspto-grants-1991_06
Patent number
US05026850

Reaction notes

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