Hydrochloric Acid → HCID 178527952, compound

HRID 876086Notes

Reaction equation

HRID 876086 reaction equation
[OH-].[K+].[NH:3]1[CH:7]=[CH:6][CH:5]=[C:4]1[C:8]([NH:10][NH2:11])=[O:9].[C:12](=S)=[S:13].Cl>CO>[NH:3]1[CH:7]=[CH:6][CH:5]=[C:4]1[C:8]1[O:9][C:12]([SH:13])=[N:11][N:10]=1

Participants

6

Procedure

Potassium hydroxide (4.78 g, 85.3 mmol) was solved in methanol (125 ml). 1H-pyrrole-2-carbohydrazide (Compound C) (9.7 g, 77.5 mmol) was added and the mixture was stirred for 30 minutes. Carbon disulfide (14.7 g, 193.8 mmol) was added to the mixture followed by stirring at 65° C. for 15 h. Another equivalent of carbon disulfide (5.90 g, 77.5 mmol) was added followed by stirring at 65° C. for 4 days. Aqueous hydrochloric acid (1 M) was added in excess quantity, the mixture was stirred and filtered and washed with aqueous hydrochloric acid. Yield 10 g (77%).

Workup

  1. stirringby stirring at 65° C. for 15 h
  2. stirringby stirring at 65° C. for 4 days
  3. stirringthe mixture was stirred
  4. filtrationfiltered
  5. washwashed with aqueous hydrochloric acid

Sources & evidence

ORD record
ord-047de9f434e6471b84531b0e35c1b880
Source dataset
uspto-grants-2015_03
Patent number
US08986654B2

Reaction notes

Loading…