Ammonium Hydroxide → HCID 14183120, compound

HRID 845442Notes

Reaction equation

HRID 845442 reaction equation
[SH:1][C:2]1[S:6][N:5]=[C:4]([C:7]2[CH:12]=[CH:11][CH:10]=[CH:9][CH:8]=2)[N:3]=1.[O-]Cl.[Na+].[OH-].[NH4+:17]>[OH-].[Na+].O>[C:7]1([C:4]2[N:3]=[C:2]([S:1][NH2:17])[S:6][N:5]=2)[CH:12]=[CH:11][CH:10]=[CH:9][CH:8]=1

Participants

6

Reactant 3

HCID 14923Ammonium HydroxideHCID 23665760Sodium HypochloriteHCID 178527832HCID 178527832, compound

Product 1

HCID 14183120HCID 14183120, compound

Reagents, catalysts & solvents 2

HCID 962WaterSolventHCID 14798Sodium HydroxideSolvent

Procedure

A solution of 30 g of 5-mercapto-3-phenyl-1,2,4-thiadiazole in 500 ml of 5% sodium hydroxide and a solution prepared by diluting 310 ml of 5.25% NaOCl to 500 ml with water were added dropwise simultaneously to 1325 ml of an ammonium hydroxide solution while maintaining the mixture at 0° with an ice/methanol bath. The resulting mixture was stirred for 10 minutes and the solids were collected, washed with water and dried under high vacuum (with P2O5) to give 18.5 g of powder. Recrystallization of 8.2 g of this material from benzene (300 ml) gave 4.8 g of crystals, m.p.>142° dec.

Workup

  1. temperaturewhile maintaining the mixture at 0° with an ice/methanol bath
  2. customthe solids were collected
  3. washwashed with water
  4. dry with materialdried under high vacuum (with P2O5)

Sources & evidence

ORD record
ord-788cbd68238f4a4696fcaf88961ebfa8
Source dataset
uspto-grants-1988_07
Patent number
US04758578

Reaction notes

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