HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → HCID 178523766, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | 2-Chloro-5-(trifluoromethyl)benzoyl chloride | HCID 2778106 | — |
| Reactant | HCID 178511559 | HCID 178511559 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 178523766 | HCID 178523766 | — |
Reaction Steps
To a solution of cis-(4-Amino-cyclohexyl)-methanol (Tetrahedron Lett., 1970, 11, 4285-4288) (0.75 g, 5.80 mmol) in THF (10 ml) is added water (1.8 mL), triethylamine (2.023 mL, 14.51 mmol) and 2-chloro-5-(trifluoromethyl)benzoyl chloride (1.411 g, 5.80 mmol). The RM is stirred at RT for 1 hour. The reaction mixture is partitioned between EtOAc and water. The organic phase is washed successively with water, saturated sodium bicarbarbonate and saturated brine, dried over MgSO4, filtered and the solvent removed in vacuo. Purification by chromatography on a pre-packed silica gel column using 0-100% EtOAc in isohexane gradient elution gave the desired product as a colourless solid.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08273900B2 |
| Source dataset | uspto-grants-2012_09 |
| ORD ID | ord-915c8295fd5b49b69c681ccff0e55fae |
| Source note | uspto-grants-2012_09 |