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Triethylamine → Toluene 4-thiosulfonic acid S-[2-tert-butyl-4-(2-methoxymethoxy-ethoxy)-5-methyl-phenyl] ester
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | 4-Methylbenzene-1-sulfonyl bromide | HCID 10130885 | — |
| 反応物 | 2-Tert-butyl-4-(2-methoxymethoxy-ethoxy)-5-methyl-benzenethiol | HCID 18798700 | — |
| 溶媒 | 1,1,2-Trichloroethane | HCID 6574 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 生成物 | Toluene 4-thiosulfonic acid S-[2-tert-butyl-4-(2-methoxymethoxy-ethoxy)-5-methyl-phenyl] ester | HCID 53987067 | — |
反応手順
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).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05834506 |
| 出典データセット | uspto-grants-1998_11 |
| ORD ID | ord-295045b58ba843feb787f80e37f1aa1e |
| 出典メモ | uspto-grants-1998_11 |