Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Chloroform | HCID 6212 | — |
| Reactant | Trifluoroacetic acid | HCID 6422 | — |
| Reactant | Potassium Carbonate | HCID 11430 | — |
| Reactant | HCID 58276276 | HCID 58276276 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 58276466 | HCID 58276466 | — |
Reaction Steps
To a solution of 1,1-dimethylethyl {2-[4′-(aminocarbonyl)-3-biphenylyl]ethyl}-carbamate (1.81 g, 0.005 mol) in CH2Cl2 (50 mL) at room temperature was added trifluoroacetic acid (15 mL) in one portion. After 1 hr the mixture was cooled in an ice bath and 1M K2CO3 (200 mL) and chloroform were added. The aqueous phase was extracted several times with mixtures of ethyl acetate, dichloromethane and chloroform. Residual solids were collected by filtration, affording the title compound as a white solid; LC/MS (method A) 1.04 min; m/z 241 (M+H). Combined organic extracts were dried over Na2SO4 and concentrated in vacuo affording an additional batch of the title compound (combined with the solid collected above). This product was used without further purification.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US08633175B2 |
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| Source dataset | uspto-grants-2014_01 |
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| ORD ID | ord-6595173633d74b31b642721006913888 |
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| Source note | uspto-grants-2014_01 |
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