Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Sodium Hydroxide | HCID 14798 | — |
| Reactant | HCID 86675423 | HCID 86675423 | — |
| Solvent | Methanol | HCID 887 | — |
| Product | HCID 67323495 | HCID 67323495 | — |
Reaction Steps
In a 500 mL 3-neck round bottom flask equipped with reflux condenser, addition funnel, thermometer socket and magnetic bar inside was added N-[5-(5-Bromo-2-methoxybenzenesulfonyl)-2-methoxyphenyl]-2,2,2-trifluoroacetamide (18.0 grams, 38.54 mmol) in methanol (200 mL). The contents of the flask were cooled to 5° C. and 6N sodium hydroxide (3.1 grams dissolved in 12.4 mL) solution (3.1 grams, 77 mmol) was added slowly over a period of 30 minutes at 5° C. The reaction mass was bought to room temperature and refluxed the reaction mass for 3 hours at 70° C. Reaction mass was cooled to room temperature and methanol was evaporated under vacuum and the obtained residue was treated with water (50 mL) and the mass was extracted with ethyl acetate (3×100 mL). The combined organic layers were washed with brine solution and dried over anhydrous sodium sulfate. Solvent was removed under reduced pressure to obtain technical product and it was further purified by recrystallisation from methanol/n-hexane to obtain the title product. Yield: 2.85 grams
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| Patent number | US09018231B2 |
|---|
| Source dataset | uspto-grants-2015_04 |
|---|
| ORD ID | ord-dc612d225d4743848293914ab2ac259a |
|---|
| Source note | uspto-grants-2015_04 |
|---|