Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Acetic Acid | HCID 176 | — |
| Reactant | Sulfuric Acid | HCID 1118 | — |
| Reactant | Sodium Hydroxide | HCID 14798 | — |
| Reactant | 1055306-54-1 | HCID 59586722 | — |
| Product | HCID 59586742 | HCID 59586742 | — |
Reaction Steps
2.75 g (17.7 mmol) of the product from example 48A are dissolved in 12 ml of glacial acetic acid and admixed with 4 ml of concentrated sulfuric acid. The mixture is heated to 130° C. for 30 min and, after cooling, stirred into ice-water. A pH of 8 is established with sodium hydroxide solution, and then extraction is effected with dichloromethane. The combined organic phases are dried over sodium sulfate and concentrated cautiously. This affords 3.30 g (94% of theory) of the title compound, which is converted further without purification.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US08198267B2 |
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| Source dataset | uspto-grants-2012_06 |
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| ORD ID | ord-6843322b8014429680fa5a07fc455713 |
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| Source note | uspto-grants-2012_06 |
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