Sulfuric Acid → HCID 18930975, compound

HRID 1599210Notes

Reaction equation

HRID 1599210 reaction equation
[F:1][S:2]([C:5]1[S:6][C:7](Cl)=[C:8]([N+:10]([O-:12])=[O:11])[CH:9]=1)(=[O:4])=[O:3].C1N2CN3CN(C2)C[N:15]1C3.S(=O)(=O)(O)O>CO>[F:1][S:2]([C:5]1([NH2:15])[CH2:9][C:8]([N+:10]([O-:12])=[O:11])=[CH:7][S:6]1)(=[O:4])=[O:3]

Participants

5

Reactant 3

HCID 1118Sulfuric AcidHCID 4101HexamethylenetetramineHCID 18930898HCID 18930898, compound

Product 1

HCID 18930975HCID 18930975, compound

Reagents, catalysts & solvents 1

HCID 887MethanolSolvent

Procedure

The 2-fluorosulphonyl-4-nitro-5-chlorothiophene (20.4 parts), was added to methanol (240 parts) with hexamine (22.5 parts). Heated to reflux and stirred under these conditions for 4 hours. Cooled to room temperature and poured onto 10% sulphuric acid solution (250 parts). The product was extracted out with ethyl acetate, separated and dried over magnessium sulphate, then screened and concentrated to yield the product 2-fluorosulphonyl-4-nitro-2-aminothiophene (16 parts).

Workup

  1. temperatureHeated
  2. temperatureto reflux
  3. extractionThe product was extracted out with ethyl acetate
  4. customseparated
  5. dry with materialdried over magnessium sulphate
  6. concentrationconcentrated

Sources & evidence

ORD record
ord-289fd91451bc477b9e6a8ef6ae0138e1
Source dataset
uspto-grants-1998_04
Patent number
US05739299

Reaction notes

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