Ammonia → HCID 21537760, compound

HRID 1076608Notes

Reaction equation

HRID 1076608 reaction equation
[CH3:1][N:2](C(=O)C)[C:3]1[S:4][CH:5]=[CH:6][C:7]=1[C:8](=[O:16])[C:9]1[CH:14]=[CH:13][CH:12]=[CH:11][C:10]=1[F:15].Cl.N>C(O)C>[CH3:1][NH:2][C:3]1[S:4][CH:5]=[CH:6][C:7]=1[C:8](=[O:16])[C:9]1[CH:14]=[CH:13][CH:12]=[CH:11][C:10]=1[F:15]

Participants

5

Reactant 3

HCID 222AmmoniaHCID 313Hydrochloric AcidHCID 21537747HCID 21537747, compound

Product 1

HCID 21537760HCID 21537760, compound

Reagents, catalysts & solvents 1

HCID 702EthanolSolvent

Conditions

Temperature
90 °C

Procedure

To a solution of 2.5 g of N-methyl-2-acetylamino-3-(o-fluorobenzoyl)thiophene in 12.5 ml of ethanol, is added 6.6 ml of 6 N aqueous hydrochloric acid. The mixture is heated at 90°C for 3 hours. After cooling, the reaction mixture is neutralized with aqueous ammonia, then extracted with ether. The ether extracts are washed with water, dried over sodium sulfate, then evaporated under reduced pressure to give an oil, which is crystallized from ethanol to give 2-methylamino-3-(o-fluorobenzoyl)thiophene as crystals having a melting point of 184.5° - 186°C.

Workup

  1. temperatureAfter cooling
  2. extractionextracted with ether
  3. washThe ether extracts are washed with water
  4. dry with materialdried over sodium sulfate
  5. customevaporated under reduced pressure
  6. customto give an oil, which
  7. customis crystallized from ethanol

Sources & evidence

ORD record
ord-dec73cd41fcb46a5972148e6511ed5ae
Source dataset
uspto-grants-1976_05
Patent number
US03957783

Reaction notes

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