HuagongsheHuagongshe Chemistry Print Report · For research reference only
Thioglycolic Acid → [{(6-Methyl-1,3-benzodioxol-5-yl)methyl}thio]acetic acid
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Thioglycolic Acid | HCID 1133 | — |
| Reactant | Sodium Hydroxide | HCID 14798 | — |
| Reactant | 5-(Chloromethyl)-6-methylbenzo[d][1,3]dioxole | HCID 10559416 | — |
| Solvent | Ethanol | HCID 702 | — |
| Product | [{(6-Methyl-1,3-benzodioxol-5-yl)methyl}thio]acetic acid | HCID 14514915 | 20.5% |
Reaction Steps
A suspension of 6.0 g of 5-chloromethyl-6-methyl-1,3-benzodioxole, 6.0 g of mercaptoacetic acid and 6.5 g of sodium hydroxide in 130 ml of 50% aqueous ethanol was heated under reflux for one hour and concentrated, followed by the addition of water. The mixture was washed with ethyl acetate. The aqueous layer was acidified with 1N hydrochloric acid and extracted with chloroform. The organic layer was dried over magnesium sulfate and distilled to remove the solvent. The residue was chromatographed over a silica gel column and eluted with chloroform to obtain a crude crystal. This crude crystal was recrystallized from diisopropyl ether to obtain 1.6 g of the title compound as a colorless crystal.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05110956 |
| Source dataset | uspto-grants-1992_05 |
| ORD ID | ord-b08da20ec3d945d0ae2b465b2de90f13 |
| Source note | uspto-grants-1992_05 |