HuagongsheHuagongshe Chemistry Print Report · For research reference only
Triethylamine → Toluene 4-thiosulfonic acid S-[2-tert-butyl-4-(2-methoxymethoxy-ethoxy)-5-methyl-phenyl] ester
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | 4-Methylbenzene-1-sulfonyl bromide | HCID 10130885 | — |
| Reactant | 2-Tert-butyl-4-(2-methoxymethoxy-ethoxy)-5-methyl-benzenethiol | HCID 18798700 | — |
| Solvent | 1,1,2-Trichloroethane | HCID 6574 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Product | Toluene 4-thiosulfonic acid S-[2-tert-butyl-4-(2-methoxymethoxy-ethoxy)-5-methyl-phenyl] ester | HCID 53987067 | — |
Reaction Steps
A solution of tosyl bromide (21.0 g; 89.32 mmol), 50 mL of trichloroethane and 20 mL of NEt3 was cooled to 0° C. To this solution was added slowly a solution of 12.4 mmol of 2-tert-butyl-4-(2-methoxymethoxy-ethoxy)-5-methyl-benzenethiol (prepared in Example AAAA) in 100 mL of trichloroethane. After 13 hours, the reaction mixture was diluted with EtOAc and washed with brine. The product was purified by flash silica gel chromatography, eluting with EtOAc:hexane (5:95, then switching to 3:7).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06046355 |
| Source dataset | uspto-grants-2000_04 |
| ORD ID | ord-3a08b547aca54d118ec6372c114765cd |
| Source note | uspto-grants-2000_04 |