HuagongsheHuagongshe Chemistry Print Report · For research reference only
2-Chloro-4-fluoro-5-nitro-thiolbenzoic acid (methoxycarbonylmethyl) ester → 5-Amino-2-chloro-4-fluoro-thiolbenzoic acid (methoxycarbonylmethyl) ester
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 2-Chloro-4-fluoro-5-nitro-thiolbenzoic acid (methoxycarbonylmethyl) ester | HCID 86746024 | — |
| Reactant | HCID 178418361 | HCID 178418361 | — |
| Catalyst | Nickel | HCID 935 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | 5-Amino-2-chloro-4-fluoro-thiolbenzoic acid (methoxycarbonylmethyl) ester | HCID 86746023 | 89.9% |
Reaction Steps
10.4 g of the 2-chloro-4-fluoro-5-nitro-thiolbenzoic acid (methoxycarbonylmethyl) ester obtained in accordance with Example P1 are hydrogenated with hydrogen under normal pressure in 150 ml of tetrahydrofuran at a temperature of 20°-25° C. in the presence of 2 g of Raney nickel catalyst. After the stoichiometric amount of hydrogen has been consumed, the catalyst is separated off and the solution is concentrated by evaporation, yielding 8.6 g of 5-amino-2-chloro-4-fluoro-thiolbenzoic acid (methoxycarbonylmethyl) ester having a melting point of from +88° to +89° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05229514 |
| Source dataset | uspto-grants-1993_07 |
| ORD ID | ord-8fae56a1f18d44f69cded735b913f272 |
| Source note | uspto-grants-1993_07 |