化工社化工社 化学情報印刷レポート · 研究参考用
Water → 1,3,5-Trimethyl-2,4-bis-(2,2,2-trifluoro-1-p-tolyl-1-trifluoromethylethoxy-sulfonyl)-benzene
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Sodium hydride | HCID 24758 | — |
| 反応物 | 2-(p-Tolyl)hexafluoroisopropanol | HCID 74829 | — |
| 反応物 | 2,4-Mesitylenedisulfonyl Dichloride | HCID 3620081 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 1,3,5-Trimethyl-2,4-bis-(2,2,2-trifluoro-1-p-tolyl-1-trifluoromethylethoxy-sulfonyl)-benzene | HCID 19700285 | — |
反応手順
7.75 g (30 mmol) of 1,1,1,3,3,3-hexafluoro-2-p-tolylpropan-2-ol were dissolved in 45 ml of DMF, and 1.2 g (40 mmol) of NaH (80% strength dispersion in mineral oil) were added. After a clear solution had formed, 5.0 g (14 mmol) of 2,4,6-trimethylbenzene-1,3-disulfonyl chloride were added and the mixture was stirred for a further 72 hours at room temperature. The mixture was poured into water and the precipitated product was filtered off and dried. 7.8 g of 1,3,5-trimethyl-2,4-bis-(2,2,2-trifluoro-1-p-tolyl-1-trifluoromethylethoxy-sulfonyl)-benzene were obtained (colorless crystals, m.p.: 178° C. [from acetonitrile]).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05716756 |
| 出典データセット | uspto-grants-1998_02 |
| ORD ID | ord-b66eebdf74734621acbce13e2060fdb5 |
| 出典メモ | uspto-grants-1998_02 |