Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | Dimethylsulphamoyl chloride | HCID 83372 | — |
| Reactant | HCID 10061288 | HCID 10061288 | — |
| Solvent | Pyridine | HCID 1049 | — |
| Product | HCID 14305467 | HCID 14305467 | 33.4% |
Reaction Steps
A mixture of 4'-amino-3'-(2,4-difluorophenoxy)acetophenone (2.0 g) and dimethylsulfamoyl chloride (11 g) in pyridine (20 ml) was stirred for 11 hours at 80° C. After cooling, the reaction mixture was poured into 2N aqueous solution of hydrochloric acid (200 ml) and extracted with ethyl acetate. The extract was washed with water, dried, and concentrated in vacuo. The residue was purified by column chromatography on silica gel (100 g) eluting with a mixture of toluene and ethyl acetate (20:1), and recrystallized from a mixture of ethanol and water (2:1, 15 ml) to give prisms of 3'-(2,4-difluorophenoxy)-4'-(dimethylsulfamoylamino)acetophenone (0.94 g).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US04866091 |
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| Source dataset | uspto-grants-1989_09 |
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| ORD ID | ord-3bd93a82819c425bbce2dd6c58ec38fa |
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| Source note | uspto-grants-1989_09 |
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