HuagongsheHuagongshe Chemistry Print Report · For research reference only
HCID 21262890, compound → HCID 21262937, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | HCID 21262890 | HCID 21262890 | — |
| Solvent | Trifluoroacetic acid | HCID 6422 | — |
| Product | HCID 21262937 | HCID 21262937 | 77% |
Reaction Steps
A solution of 6.3 g of (E)-2-[1-(4-t-butylaminosulphonylphenyl)-1-(3-fluoro-4-methylphenyl)methylidene]butane-1,4-diol prepared in Example 138 in 75 ml of trifluoroacetic acid is heated for 10 hours under reflux. The solvent is concentrated under vacuum and the residue is taken up in a dilute solution of sodium hydroxide, washed with dichloromethane and then acidified with dilute hydrochloric acid and extracted with dichloromethane. The organic phases are combined and dried over magnesium sulphate and then evaporated under vacuum. The residue is crystallised in tert-butyl methyl ether to give 4 g of (E)-4-[(3-fluoro-4-methylphenyl)-(tetrahydro-furan-3-ylidene)methyl]benzenesulphonamide in the form of crystals melting at 174-176° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06180651B2 |
| Source dataset | uspto-grants-2001_01 |
| ORD ID | ord-09f1226951ba4c1b9f7fe397b011adf7 |
| Source note | uspto-grants-2001_01 |