Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Ammonia | HCID 222 | — |
| Reactant | HCID 10024618 | HCID 10024618 | — |
| Solvent | 1-Butanol | HCID 263 | — |
| Solvent | Methanol | HCID 887 | — |
| Product | HCID 10340604 | HCID 10340604 | 38% |
Reaction Steps
A mixture of the thioamide (from Example 19) (2.98 g, 7.24 mmol) and red mercuric oxide (1.57 g, 7.24 mmol) in n-butanol (40 ml) was saturated with ammonia gas at room temperature, and then stirred at 120° C. for 3 hours. After being cooled, the mixture was diluted with methanol (150 ml) and filtered through Arbocel filter aid. The filtrate was concentrated under reduced pressure, and the residue was purified by flash chromatography (eluting with ethyl acetate:methanol:diethylamine=100:10:5). Fractions containing the product were evaporated to give the title compound as a bright yellow solid (1.085 g, 38%), m.p. 299°-302° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US05008263 |
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| Source dataset | uspto-grants-1991_04 |
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| ORD ID | ord-122b88e4a45f443db0f15df5d3f2cd90 |
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| Source note | uspto-grants-1991_04 |
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