HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → HCID 24808477, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | Diethyl Ether | HCID 3283 | — |
| Reactant | HCID 24989972 | HCID 24989972 | — |
| Solvent | 1,4-Dioxane | HCID 31275 | — |
| Product | HCID 24808477 | HCID 24808477 | 75% |
Reaction Steps
To a solution of tert-butyl[(2S)-3-phenyl-2-({[1-(2,2,2-trifluoroethyl)-4,5-dihydro-1H-pyrrolo[2,3-f]isoquinolin-3-yl]carbonyl}amino)propyl]carbamate L8 (0.38 mmol) in dry dioxane (20 mL), 4M HCl in dioxane (5 mL) was added. The reaction mixture was stirred at rt overnight. The solvent was removed and the residue dissolved with DCM and washed with aq NaHCO3. The organic layer was dried (Na2SO4) and concentrated. Purification by chromatography on silica gel (eluant: DCM/MeOH 19:1) gave, after trituration with diethylether, the title compound (75% yield). ESI (+) MS: m/z 429 (MH+). 1H-NMR: 4.06-4.18 (m, 1H), 5.32 (q, J=8.98, 2H), 7.18 (m, 1H), 7.48 (d, J=5.24, 1H), 7.57 (s, 1H), 7.71 (d, J=8.41, 1H), 8.38 (d, J=5.24, 1H), 8.40 (s, 1H).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08207180B2 |
| Source dataset | uspto-grants-2012_06 |
| ORD ID | ord-096e007ffe9a411ab14258a6ee5a4aaf |
| Source note | uspto-grants-2012_06 |