HuagongsheHuagongshe Chemistry Print Report · For research reference only
Triethylamine → HCID 6467323, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | 4-Fluorobenzyl chloride | HCID 9602 | — |
| Reactant | 1,4-Dioxa-8-azaspiro(4.5)decane | HCID 67435 | — |
| Solvent | Chloroform | HCID 6212 | — |
| Product | HCID 6467323 | HCID 6467323 | 94% |
Reaction Steps
1,4-Dioxa-8-azaspiro[4.5]decane (29.9 g) was dissolved in chloroform (150 ml), triethylamine (32 ml) and p-fluorobenzyl chloride (27.5 ml) were successively added under ice-cooling, and the mixture was stirred overnight. The reaction solution was successively washed with a 20% aqueous solution of sodium hydroxide (150 ml×2) and water (150 ml), dried over anhydrous magnesium sulfate, and the solvent was distilled off under reduced pressure. The residue obtained was purified by silica gel column chromatography (chloroform:methanol=10:1) to give the title compound (49.4g) as a yellow oily substance. Yield=94%.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05945434 |
| Source dataset | uspto-grants-1999_08 |
| ORD ID | ord-b3e96b380f114466b4f1ac1b07723bec |
| Source note | uspto-grants-1999_08 |