Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Pyridine | HCID 1049 | — |
| Reactant | 2,2,2-Trichloroethyl chloroformate | HCID 87063 | — |
| Reactant | Benzoic acid, 4-[(4-amino-3-fluorophenyl)thio]-3-nitro-, methyl ester | HCID 67040417 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 67041134 | HCID 67041134 | 94% |
Reaction Steps
The product of Example 96B (2.0 g, 6.2 mmol) and pyridine (0.55 mL, 6.8 mmol) in CH2Cl2 (20 mL) was reacted with 2,2,2-trichloroethyl chloroformate (0.92 mL, 6.5 mmol) dropwise at 5° C. The mixture was stirred at 5° C. for 30 minutes and concentrated. The residue was diluted with water (50 mL). The resulting crystals were collected by filtration, washed with water and i-Pr2O, and dried at room temperature in vacuum overnight to give the title compound as pale yellow crystals (2.9 g, 93%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| Patent number | US08236950B2 |
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| Source dataset | uspto-grants-2012_08 |
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| ORD ID | ord-8ce8616f1c8141da97a59eba48903609 |
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| Source note | uspto-grants-2012_08 |
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