Potassium Hydroxide → HCID 178526578, compound

HRID 252992

Reaction equation

HRID 252992 reaction equation
[SH-:1].[C+4:2].[SH-:3].[SH-].[SH-].[N+:6]([C:9]1[CH:18]=[CH:17][CH:16]=[CH:15][C:10]=1[C:11]([NH:13][NH2:14])=O)([O-:8])=[O:7].[OH-].[K+]>CO>[N+:6]([C:9]1[CH:18]=[CH:17][CH:16]=[CH:15][C:10]=1[C:11]1[S:1][C:2]([SH:3])=[N:14][N:13]=1)([O-:8])=[O:7]

Participants

5

Reactant 3

HCID 14797Potassium HydroxideHCID 3781218o-NitrobenzohydrazideHCID 178420937HCID 178420937, compound

Product 1

HCID 178526578HCID 178526578, compoundYield 51%

Reagents, catalysts & solvents 1

HCID 887MethanolSolvent2×

Procedure

Carbon bisulfide (4 ml) was added to a solution of 1.81 g (10 mmol) of 2-nitrobenzohydrazide in 8 ml of methanol. A solution of 616 mg (11 mmol) of potassium hydroxide in methanol (10 ml) was added thereto, and the mixture was stirred at room temperature for 6 hr. The precipitated crystal was collected by filtration and was dried. The dried crystal was added dropwise to 5 ml of concentrated sulfuric acid, and the mixture was stirred at room temperature for 3 hr. The reaction solution was added dropwise to 100 ml of ice water, and the resultant precipitate was collected by filtration and was dried to give 1.21 g (51%) of the title compound.

Workup

  1. filtrationThe precipitated crystal was collected by filtration
  2. customwas dried
  3. additionThe dried crystal was added dropwise to 5 ml of concentrated sulfuric acid
  4. stirringthe mixture was stirred at room temperature for 3 hr
  5. additionThe reaction solution was added dropwise to 100 ml of ice water
  6. filtrationthe resultant precipitate was collected by filtration
  7. customwas dried

Sources & evidence

ORD record
ord-605d4926122c4a8a9888895ae597d2ec
Source dataset
uspto-grants-2011_01
Patent number
US07871982B2

Linked notes

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