HuagongsheHuagongshe Chemistry Print Report · For research reference only
Chloroacetaldehyde → HCID 11667810, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Chloroacetaldehyde | HCID 33 | — |
| Reactant | HCID 11631574 | HCID 11631574 | — |
| Solvent | Acetic Acid | HCID 176 | — |
| Solvent | Water | HCID 962 | — |
| Product | HCID 11667810 | HCID 11667810 | — |
Reaction Steps
to 2-[3-(3,4-Dichloro-phenoxy)-8-aza-bicyclo[3.2.1]oct-8-yl]-thioacetamide (0.5 g) in 5 ml of acetic acid was added 0.13 g of 50% chloroacetaldehyde in water. The reaction mixture was stirred at reflux overnight and cooled to room temperature and poured into 50 ml of water. The mixture was extracted twice with dichloromethane. The organic phase was dried with magnesium sulphate and evaporated to and oil. The product was isolated by column chromatography with dichloromethane/methanol (9:1) with 1% ammonia as eluent, the product fractions was evaporated to dryness. Yield 0.1 g (19%). Mp. 123-124° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07713990B2 |
| Source dataset | uspto-grants-2010_05 |
| ORD ID | ord-713e794d8e104a99b415333117005595 |
| Source note | uspto-grants-2010_05 |