HuagongsheHuagongshe Chemistry Print Report · For research reference only
Methanol → HCID 178424414, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Methanol | HCID 887 | — |
| Reactant | Cyanomethylenetributylphosphorane | HCID 4622928 | — |
| Reactant | HCID 178424415 | HCID 178424415 | — |
| Solvent | Toluene | HCID 1140 | — |
| Product | HCID 178424414 | HCID 178424414 | 29.4% |
Reaction Steps
A mixture of 41 mg (0.1 mmol) N-{trans-4-[(4-isopropylpiperazin-1-yl)carbonyl]cyclohexyl}-2-methylbenzenesulfonamide (example 4), 72 mg (0.3 mmol) cyanomethylene tri-n-butylphosphorane and 32 mg (1 mmol) methanol in 2 mL toluene was heated for 16 h to 110° C. After evaporation methanol and DMF were added and the mixture was subjected to preparative HPLC purification on reversed phase eluting with a gradient of acetonitrile/water (0.1% NEt3). The combined product fractions were evaporated to dryness to yield 12.4 mg (29%) of the title compound. MS (m/e): 422.2 (MH+).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08017773B2 |
| Source dataset | uspto-grants-2011_09 |
| ORD ID | ord-c2c5eff67ae941fb9797ccca0317d574 |
| Source note | uspto-grants-2011_09 |