Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Sulfamic Acid | HCID 5987 | — |
| Reactant | HCID 22009524 | HCID 22009524 | — |
| Reactant | Sodium Chlorite | HCID 23668197 | — |
| Solvent | Acetic Acid | HCID 176 | — |
| Solvent | Water | HCID 962 | — |
| Product | HCID 18403995 | HCID 18403995 | — |
Reaction Steps
A solution of 0.88 g of sodium chlorite in 5 ml of water is added dropwise to 1.6 g of 7-difluoromethoxy-2-(1-methylethyl)benzofuran-4-carbaldehyde and 0.83 g of amidosulfuric acid, dissolved in 15 ml of glacial acetic acid, such that the internal temperature is kept between 15 and 20° C. The mixture is stirred for a further 1 h and then poured into 150 ml of ice water, and the precipitate formed is filtered off with suction and washed with water until acid-free. For purification, the crude product is dissolved in halfconcentrated, aqueous ammonia, and the aqueous solution is extracted with toluene and acidified with 2 N hydrochloric acid to pH 1-2. The precipitate formed is filtered off with suction, washed with water until acid-free and dried in vacuo: m.p. 169° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US06020340 |
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| Source dataset | uspto-grants-2000_02 |
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| ORD ID | ord-4cf21c5502a04bfe8ed5d973983be9e6 |
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| Source note | uspto-grants-2000_02 |
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