HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → HCID 15858644, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | HCID 15858642 | HCID 15858642 | — |
| Reactant | 8,8,9,9,9-Pentafluoro-nonyltosylate | HCID 23497152 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 15858644 | HCID 15858644 | — |
Reaction Steps
A solution of 1.77 g of 11β-fluoro-7α-[5-(methyl-amino)-pentyl]-estra-1,3,5(10)-triene-3,17β-diol in 18 ml of dimethylformamide is stirred with 1.4 g of 8,8,9,9,9-pentafluoro-nonyltosylate for 1 hour at a bath temperature of 80° C. Then, it is added to water, extracted three times with ethyl acetate, washed with water and common salt solution, dried on sodium sulfate, concentrated by evaporation in a vacuum and chromatographed on silica gel with dichloromethane/methanol. 11β-Fluoro-7α-{5-[methyl-(8,8,9,9,9-pentafluoro-nonyl)-amino]-pentyl}-estra-1,3,5(10)-triene-3,17β-diol is obtained as crystals with a melting point of 110° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06780855B2 |
| Source dataset | uspto-grants-2004_08 |
| ORD ID | ord-32e66745a8314835a06ef076e64e5c39 |
| Source note | uspto-grants-2004_08 |