化工社化工社 化学情報印刷レポート · 研究参考用
Trifluoroacetic acid → (2-Bromophenyl)(2,4,6-trimethoxybenzyl)sulfane
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Trifluoroacetic acid | HCID 6422 | — |
| 反応物 | 2-Bromobenzenethiol | HCID 80598 | — |
| 反応物 | Sodium Bicarbonate | HCID 516892 | — |
| 反応物 | 2,4,6-Trimethoxybenzyl alcohol | HCID 602515 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | (2-Bromophenyl)(2,4,6-trimethoxybenzyl)sulfane | HCID 66870845 | 89% |
反応手順
To a solution of 30.8 g (2,4,6-trimethoxyphenyl)methanol (155.4 mmol) and 29.2 g 2-bromobenzenethiol (155.4 mmol) in 150 ml DCM at 0° C. was added dropwise 1.3 eq TFA. The reaction was stirred 15 minutes at room temperature before saturated NaHCO3 was added until neutral. The organic volatiles were removed under reduced pressure and the aqueous residue was extracted with ethyl acetate (3×150 ml). The organic layer was collected, washed with brine and dried over magnesium sulfate, filtered, and concentrated under reduced pressure afforded a yellowish solid. The solid was washed with ethyl acetate to yield 51.3 g white solid (2-bromophenyl)(2,4,6-trimethoxybenzyl)sulfane (13.9 mmol, 89% yield).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07550505B2 |
| 出典データセット | uspto-grants-2009_06 |
| ORD ID | ord-399fea0165bb4c1f8fcb279647e96072 |
| 出典メモ | uspto-grants-2009_06 |