Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | Heptane | HCID 8900 | — |
| Reactant | Potassium Hydroxide | HCID 14797 | — |
| Reactant | HCID 66973773 | HCID 66973773 | — |
| Solvent | Ethanol | HCID 702 | — |
| Solvent | Water | HCID 962 | — |
| Product | HCID 53348247 | HCID 53348247 | — |
Reaction Steps
N-[4-(2-methylsulfamoyl-ethyl)-2-trimethylsilanylethynyl-phenyl]-acetamide (100 g) was dissolved in ethanol (1000 ml) at 25° C. and cooled to 15-20° C. Potassium hydroxide (20 gm) was added slowly maintaining temperature below 25° C., stirred for 2-3 hours and cooled to 10-15° C. pH of the reaction mixture was adjusted to 5 with 10% dilute HCl and concentrated under vacuum below 40° C. to obtain a residue. The residue was dissolved in water (250 ml) and extracted with dichloromethane (2000 ml). The organic layer was washed with water and concentrated under vacuum to obtain a residue. The residue was treated with heptane (200 ml) to obtain a solid which was filtered and dried under vacuum at 50-55° C. for 12 hours. (Yield: 70 g, HPLC Purity: 99%)
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US08735589B2 |
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| Source dataset | uspto-grants-2014_05 |
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| ORD ID | ord-1dcf2b84f10844ac9a488c430f0a6f22 |
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| Source note | uspto-grants-2014_05 |
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