HuagongsheHuagongshe Chemistry Print Report · For research reference only
Dichloromethane → HCID 68621897, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Dichloromethane | HCID 6344 | — |
| Reactant | HCID 68620864 | HCID 68620864 | — |
| Catalyst | Titanium isopropoxide | HCID 11026 | — |
| Product | Dichloromethane methanol ammonium hydroxide | HCID 21896990 | — |
| Product | HCID 68621897 | HCID 68621897 | 96% |
Reaction Steps
Tetraisopropyl orthotitanate (7.6 mg, 27 μmol) and Bis(tricyclohexylphosphine)-benzylideneruthenium(IV)dichloride (11 mg, 13 μmol) were added to a solution of (RS,RS,RS)-[3-(acryloyl-but-3-enyl-amino)-9,10-dimethoxy-1,3,4,6,7,11b-hexahydro-2H-pyrido[2,1-a]isoquinolin-2-yl]-carbamic acid tert-butyl ester (65 mg, 0.13 mmol) in dichloromethane (2.5 mL). The reaction mixture was stirred 45 min at r.t., then partitioned between ethyl acetate and water. The organic layer was washed with brine, dried (MgSO4), and evaporated. Chromatography (SiO2, CH2Cl2/MeOH/NH4OH 95:5:0.25) afforded the title compound (59 mg, 96%). White solid, MS (ISP) 458.4 (M+H)+.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07122555B2 |
| Source dataset | uspto-grants-2006_10 |
| ORD ID | ord-8a325fb0466d405c82283c57d6929495 |
| Source note | uspto-grants-2006_10 |