HuagongsheHuagongshe Chemistry Print Report · For research reference only
Sodium Hydroxide → HCID 59164408, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Sodium Hydroxide | HCID 14798 | — |
| Reactant | Methanesulfonohydrazide | HCID 269268 | — |
| Reactant | HCID 11965697 | HCID 11965697 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 59164408 | HCID 59164408 | 94% |
Reaction Steps
A solution of CH3SO2NHNH2 (61 mg, 0.555 mmol) in THF (1 mL) was slowly added dropwise to a solution of 2-isocyanato-5-(3-methoxy-propionyl)-4-trifluoromethyl-benzoic acid methyl ester (167 mg, 0.505 mmol) in dry THF (2.6 mL). After stirring the mixture at r.t. for 105 min, aq NaOH (1 M, 0.53 mL) was added and stirring was continued for 60 min. The reaction mixture was concentrated and the residue was taken in EtOAc and washed with water. The aqueous phase was extracted with EtOAc (3×), all organic phases are combined, washed with brine and dried (Na2SO4) and the solvent was evaporated to dryness yielding the title compound (194 mg, 94%) as a white powder, mp 186-191° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08513268B2 |
| Source dataset | uspto-grants-2013_08 |
| ORD ID | ord-a34c8e3ecff144ab93b173eea7bc8f82 |
| Source note | uspto-grants-2013_08 |