HuagongsheHuagongshe Chemistry Print Report · For research reference only
Dichloromethane → HCID 68620864, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Dichloromethane | HCID 6344 | — |
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | Acryloyl chloride | HCID 13140 | — |
| Reactant | HCID 68620413 | HCID 68620413 | — |
| Product | Dichloromethane methanol ammonium hydroxide | HCID 21896990 | — |
| Product | HCID 68620864 | HCID 68620864 | 75% |
Reaction Steps
Acryloyl chloride (18 mg, 0.20 mmol) was added dropwise at 0° C. to a solution of (RS,RS,RS)-(3-but-3-enylamino-9,10-dimethoxy-1,3,4,6,7,11b-hexahydro-2H-pyrido[2,1-a]isoquinolin-2-yl)-carbamic acid tert-butyl ester (77 mg, 0.18 mmol) and triethylamine (20 mg, 0.20 mmol) in dichloromethane (1.5 mL). After 30 min at 0° C. the reaction mixture was partitioned between 2 M aq. sodium carbonate solution and ethyl acetate. The organic layer was washed with brine, dried (MgSO4), and evaporated. Chromatography (SiO2, CH2Cl2/MeOH/NH4OH 95:5:0.25) afforded the title compound (65 mg, 75%). White solid, MS (ISP) 486.5 (M+H)+.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07122555B2 |
| Source dataset | uspto-grants-2006_10 |
| ORD ID | ord-a2c982e1f27a497f9889d0337847cae5 |
| Source note | uspto-grants-2006_10 |