HuagongsheHuagongshe Chemistry Print Report · For research reference only
Benzene → HCID 14514923, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Benzene | HCID 241 | — |
| Reactant | Thioglycolic Acid | HCID 1133 | — |
| Reactant | p-Toluenesulfonic acid | HCID 6101 | — |
| Reactant | 7228-18-4 | HCID 346963 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Product | HCID 14514923 | HCID 14514923 | 77.5% |
Reaction Steps
A mixture comprising 2 g of 1-(1,3-benzodioxol-5-yl)-2-methyl-1-propanol, 1.3 g of mercaptoacetic acid, a catalytic amount of p-toluenesulfonic acid and 50 ml of benzene was heated under reflux for 5.5 hours, followed by the addition of ethyl acetate. The mixture was washed with water and extracted with a 2N aqueous solution of sodium hydroxide. The aqueous layer was washed with chloroform, acidified with dilute hydrochloric acid and extracted with ethyl acetate. The extract was washed with water, dried over anhydrous magnesium sulfate and concentrated in a vacuum to obtain a residue. This residue was purified by silica gel column chromatography (chloroform/methanol=20:1) to obtain 2.14 g of the title compound as a colorless oil.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05475024 |
| Source dataset | uspto-grants-1995_12 |
| ORD ID | ord-25a7d72f8bc14d3ca44a31204bc079a0 |
| Source note | uspto-grants-1995_12 |