HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → HCID 9950967, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | Lithium Hydroxide | HCID 3939 | — |
| Reactant | HCID 15406546 | HCID 15406546 | — |
| Reactant | Diethylether water | HCID 21584184 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 9950967 | HCID 9950967 | — |
Reaction Steps
A solution of methyl 4-(5,5,8,8-tetramethyl-5,6,7,8-tetrahydro-2-naphthylsulphanylethynyl)benzoate (590 mg, 1.6 mmol) and of lithium hydroxide (383 mg, 9.3 mmol) in THF is refluxed for 24 hours. The reaction mixture is poured into an Et2O/water mixture, acidified to pH 1 with concentrated hydrochloric acid solution, and extracted once with ethyl ether. After separation of the phases by settling, the organic phase is washed twice with water, dried over magnesium sulphate and concentrated on a rotary evaporator under vacuum at 40° C. The solid obtained is crystallized from heptane and 440 mg (77%) of a white solid are obtained. m.p. (melting point)=193.5° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06201019B1 |
| Source dataset | uspto-grants-2001_03 |
| ORD ID | ord-9c84cec01b1140608078d52ccbeae905 |
| Source note | uspto-grants-2001_03 |