HuagongsheHuagongshe Chemistry Print Report · For research reference only
Ethanol → HCID 69522441, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Ethanol | HCID 702 | — |
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | Hydrazine hydrate (1:1) | HCID 24654 | — |
| Reactant | 4-(3,4-Dichlorophenoxy)-1-piperidineethanamine | HCID 11358209 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 69522441 | HCID 69522441 | — |
Reaction Steps
To a solution of the product of Example 3, Step b (0.85 g) and triethylamine (0.82 ml) at RT in dichloromethane (20 ml) was added methyl oxalyl chloride (0.30 ml) dropwise over 10 minutes. The reaction mixture was partitioned between water (20 ml) and dichloromethane (20 ml). The organic phase was separated and dried with MgSO4. Evaporation under reduced pressure gave an oil which was dissolved in ethanol (10 ml) at RT and treated with hydrazine hydrate (1 ml) The reaction mixture was stirred at reflux for 24 hours, filtered and the filtrate evaporated under reduced pressure to leave an oil. Purification by flash chromatography (dichloromethane:methanol 90:10)gave the sub-title compound as a white solid (0.18 g).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07304077B2 |
| Source dataset | uspto-grants-2007_12 |
| ORD ID | ord-3ddb5fc434d641dcb08a4eb1c88b3666 |
| Source note | uspto-grants-2007_12 |