Hydrochloric Acid → HCID 13773281, compound

HRID 1651451Notes

Reaction equation

HRID 1651451 reaction equation
[CH3:1][S:2][C:3]1[CH:8]=[CH:7][C:6]([C:9](=[S:15])SCC(O)=O)=[CH:5][CH:4]=1.[OH-].[K+].O.[NH2:19][NH2:20].Cl>CO>[CH3:1][S:2][C:3]1[CH:8]=[CH:7][C:6]([C:9]([NH:19][NH2:20])=[S:15])=[CH:5][CH:4]=1

Participants

6

Reactant 4

HCID 313Hydrochloric AcidHCID 14797Potassium HydroxideHCID 24654Hydrazine hydrate (1:1)HCID 13773280HCID 13773280, compound

Product 1

HCID 13773281HCID 13773281, compound

Reagents, catalysts & solvents 1

HCID 887MethanolSolvent

Procedure

To a solution of the product of step c) (15.0 g) in methanol (200 ml) was added aqueous potassium hydroxide (58.0 ml, 1M) followed by hydrazine monohydrate (3.1 ml) dropwise over 30 minutes. After stirring at room temperature for 1 hour the mixture was acidified to pH 5 with concentrated hydrochloric acid. The resulting precipitate was filtered off and recrystallised from ethanol to afford the sub-title compound (9.9 g) as pale yellow plates. mp 152°-153°.

Workup

  1. filtrationThe resulting precipitate was filtered off
  2. customrecrystallised from ethanol

Sources & evidence

ORD record
ord-8ddd58ab65e24e9987d4732e62dec04c
Source dataset
uspto-grants-1990_05
Patent number
US04927822

Reaction notes

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