HuagongsheHuagongshe Chemistry Print Report · For research reference only
Potassium Hydroxide → HCID 21919474, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Potassium Hydroxide | HCID 14797 | — |
| Reactant | HCID 66692096 | HCID 66692096 | — |
| Solvent | Oxolane--water (1/1) | HCID 21881883 | — |
| Product | HCID 21919474 | HCID 21919474 | 99.4% |
Reaction Steps
Potassium hydroxide pellets (86%, 4.47 g, 68.5 mmol) was added to a suspension of (RS,RS,RS)-2-tert-butoxycarbonylamino-9,10-dimethoxy-1,3,4,6,7,11b-hexahydro-2H-pyrido[2,1-a]isoquinoline-3-carboxylic acid ethyl ester (7.44 g, 17.1 mmol) in tetrahydrofuran/water 1:1 (140 mL). After heating 5 h at reflux, the mixture was concentrated in vacuo. The residue was taken up in 1M aq. potassium phosphate buffer (pH 6.85) and dichloromethane, and ethanol was added until a clear two-phase mixture was obtained. The organic layer was separated, washed with brine and evaporated to afford the title compound (6.91 g, 99%). Light yellow solid, MS (ISP) 405.3 (M−H)−.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07122555B2 |
| Source dataset | uspto-grants-2006_10 |
| ORD ID | ord-69f9cd3856c34e398baf97b75bed088e |
| Source note | uspto-grants-2006_10 |