HuagongsheHuagongshe Chemistry Print Report · For research reference only
Lithium Hydroxide → HCID 86585474, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Lithium Hydroxide | HCID 3939 | — |
| Reactant | HCID 12071468 | HCID 12071468 | — |
| Reactant | Acetonitrile--water (1/1) | HCID 18373917 | — |
| Solvent | Water | HCID 962 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 86585474 | HCID 86585474 | 21% |
Reaction Steps
A mixture of ethyl (±)-10,11-dihydro-3-[4-(pyridin-2-ylamino)-1-butyl]-5H-dibenzo[a,d]cycloheptene-10-acetate (46 mg, 0.11 mmole) and 1.0 N LiOH (0.66 mL, 0.66 mmole) in THF (3 mL) and H2O (3 mL) was stirred at RT. After 24 hr, the reaction mixture was concentrated on the rotavap, and the residue was diluted with H2O (5 mL). The solution was cooled in an ice bath, and 1.0 N AcOH was added slowly to give a white precipitate. Chromatography on C-18 YMC (45% CH3CN/H2O containing 0.1% TFA) gave the title compound (13 mg, 21%) as a white solid: MS (ES) m/e 401.3 (M+H)+. Anal. Calcd for C26H28N2O2.0.75 H2O.1.5 CF3CO2H: C, 59.54; H, 5.31, N, 4.72. Found: C, 59.69; H, 5.31; N, 4.72.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06576643B2 |
| Source dataset | uspto-grants-2003_06 |
| ORD ID | ord-476f4a6832424f928653781d045d06f9 |
| Source note | uspto-grants-2003_06 |