HuagongsheHuagongshe Chemistry Print Report · For research reference only
HCID 11048255, compound → HCID 10870788, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | HCID 11048255 | HCID 11048255 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Solvent | Boron tribromide | HCID 25134 | — |
| Product | HCID 10870788 | HCID 10870788 | 98.3% |
Reaction Steps
To a cold solution (−78° C.) of N-[2-[(5-chloro-2-methoxyphenyl) carbonyl]-4-(trifluoromethyl) phenyl]aminocarboxylic acid, 1,1-dimethylethyl ester prepared in Example 1, Step A (7.0 g, 21.2 mmol) in methylene chloride (60 mL), 1.0 M BBr3 solution in methylene chloride (46.7 mL, 46.7 mmol) was added dropwise. The resultant red solution was allowed to warm to room temperature and stirred overnight. The reaction mixture was quenched with saturated NaHCO3 solution. The organic layer was separated and washed with water, brine and then dried (MgSO4). Evaporation of the solvent gave a yellow-reddish solid which was recrystallized from CH2Cl2/hexanes to afford the title compound as a yellow solid (6.58 g, 98%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06184231B2 |
| Source dataset | uspto-grants-2001_02 |
| ORD ID | ord-4f57afbf0a9f484cb120912a896087ee |
| Source note | uspto-grants-2001_02 |