HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → HCID 9891469, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | Sulfolane | HCID 31347 | — |
| Reactant | Thiourea | HCID 2723790 | — |
| Reactant | HCID 20245598 | HCID 20245598 | — |
| Solvent | Water | HCID 962 | — |
| Solvent | 2-Methoxyethanol | HCID 8019 | — |
| Product | HCID 9891469 | HCID 9891469 | — |
Reaction Steps
1.99 g of ethyl 3-[4-(6-acetoxy-2-isobutyl-5,7,8-trimethylchroman-2-ylmethoxy)phenyl]-2-chloropropionate, 0.42 g of thiourea and 2.1 g of sulfolane were reacted under a nitrogen stream at 125°-150° C. for 3.5 hours. At the end of this time, 15 ml of ethylene glycol monomethyl ether, 4 ml of water and 2 ml of concentrated hydrochloric acid were added and the mixture was reacted for a further 3.5 hours at 96°-98° C. The reaction mixture was then treated as described in Example 1(a) and the resulting crude product, in the form of an oil, was purified by column chromatography through silica gel, eluted with a 5:1 by volume mixture of hexane and ethyl acetate, to give the title compound.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US04572912 |
| Source dataset | uspto-grants-1986_02 |
| ORD ID | ord-753c17ae561347c29f6d01ca9f64cf67 |
| Source note | uspto-grants-1986_02 |