HuagongsheHuagongshe Chemistry Print Report · For research reference only
6-(1-Ethynylbutoxy)-7,8-difluoro-2-pentylchroman → 5,6-Difluoro-3-pentyl-8-propyl-1,2,3,8-tetrahydropyrano[3,2-f]-chromene
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 6-(1-Ethynylbutoxy)-7,8-difluoro-2-pentylchroman | HCID 58151900 | — |
| Solvent | N,N-Diethylaniline | HCID 7061 | — |
| Solvent | tert-Butyl methyl ether | HCID 15413 | — |
| Product | 5,6-Difluoro-3-pentyl-8-propyl-1,2,3,8-tetrahydropyrano[3,2-f]-chromene | HCID 58151918 | — |
Reaction Steps
9.0 g (26.8 mmol) of 6-(1-ethynylbutoxy)-7,8-difluoro-2-pentylchroman are heated at 205° C. for 3 h in 90 ml of N,N-diethylaniline. The batch is diluted with MTBE and washed a number of times with 3 N HCl. The organic phase is dried using sodium sulfate and evaporated to dryness. The residue is purified by column chromatography (SiO2, n-heptane:MTBE=4:1), giving 5,6-difluoro-3-pentyl-8-propyl-1,2,3,8-tetrahydropyrano[3,2-f]-chromene as a pale-brown oil.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08303844B2 |
| Source dataset | uspto-grants-2012_11 |
| ORD ID | ord-5ab23ce4abd542ec92b11f8b31310418 |
| Source note | uspto-grants-2012_11 |