HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → HCID 13315029, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Sodium amide | HCID 24533 | — |
| Reactant | 2,2,2-Trifluoroethyl trichloromethanesulphonate | HCID 90027 | — |
| Reactant | HCID 13308996 | HCID 13308996 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 13315029 | HCID 13315029 | — |
Reaction Steps
To 5-(morpholin-2-yl)methylidene-10,11-dihydro-5H-dibenzo[a,d]cycloheptene (0.69 g) in anhydrous tetrahydrofuran was added sodium amide (0.20 g) at room temperature, and the resulting mixture was heated under reflux for 1.5 hours. After cooling, 2,2,2-trifluoroethyl trichloromethylsulfonate (0.666 g) in annydrous tetrahydrofuran was added to the mixture under ice-cooling, and then the mixture was heated under reflux for 11.5 hours. After cooling, water (0.2 g) was added thereto and inorganic materials were eliminated by filtration. The filtrate was evaporated and chromatographed to afford 5-[4-(2,2,2-trifluoroethyl)morpholin-2-yl]methylidene-10,11-dihydro-5H-dibenzo[a,d]cycloheptene as oily material. M.P., 174° - 177° C (hydrochloride).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US04085210 |
| Source dataset | uspto-grants-1978_04 |
| ORD ID | ord-9e79adbf53e74ff0b8d0332d1b192730 |
| Source note | uspto-grants-1978_04 |