Sodium Hydroxide → HCID 178527846, compound

HRID 1071316Notes

Reaction equation

HRID 1071316 reaction equation
Br.[N:2]1[CH:7]=[CH:6][C:5]([C:8]2[N:9]=[C:10]([SH:13])[S:11][CH:12]=2)=[CH:4][CH:3]=1.[OH-].[Na+]>O>[N:2]1[CH:3]=[CH:4][C:5]([C:8]2[N:9]=[C:10]([SH:13])[S:11][CH:12]=2)=[CH:6][CH:7]=1

Participants

4

Reactant 2

HCID 14798Sodium HydroxideHCID 178419755HCID 178419755, compound

Product 1

HCID 178527846HCID 178527846, compound

Reagents, catalysts & solvents 1

HCID 962WaterSolvent

Procedure

4-(4-Pyridyl)-1,3-thiazole-2-thiol.hydrobromide (89.3 g, 0.32 mol) was suspended in water (627 mL) under a nitrogen stream, and 25% aqueous sodium hydroxide solution (110.5 g, 0.69 mol) was added for dissolution. An insoluble material was filtered and washed with water (100 mL). 35% Hydrochloric acid (31 mL) was added to the filtrate to adjust to pH 6.8. The precipitated crystals were collected by filtration, and washed with water (20 mL) and methanol (20 mL). The obtained crystals were suspended in methanol (627 mL). After stirring for 2 hr, the crystals were filtrated and dried. yield: 47.6 g (75.6%)

Workup

  1. additionwas added for dissolution
  2. filtrationAn insoluble material was filtered
  3. washwashed with water (100 mL)
  4. addition35% Hydrochloric acid (31 mL) was added to the filtrate
  5. filtrationThe precipitated crystals were collected by filtration
  6. washwashed with water (20 mL) and methanol (20 mL)
  7. filtrationthe crystals were filtrated
  8. customdried

Sources & evidence

ORD record
ord-874b7341dea44a0ca3b92e89c5fac844
Source dataset
uspto-grants-2005_06
Patent number
US06906055B2

Reaction notes

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