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2,6-Dimethylbenzoic acid → 2,6-Dimethyl-3-((2,2,2-trifluoroacetamido)methyl)benzoic acid
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 2,6-Dimethylbenzoic acid | HCID 12439 | — |
| 反応物 | 2,2,2-Trifluoro-N-(hydroxymethyl)acetamide | HCID 3084931 | — |
| 溶媒 | Sulfuric Acid | HCID 1118 | — |
| 生成物 | 2,6-Dimethyl-3-((2,2,2-trifluoroacetamido)methyl)benzoic acid | HCID 86692227 | 56,519.699% |
反応手順
To a solution of 2,6-dimethyl benzoic acid (6.8 g, 0.045 mmol) in conc. H2SO4 (100 mL), 2,2,2-trifluoro-N-(hydroxymethyl)acetamide (7.1 g, 0.049 mmol) was added and the reaction mixture was stirred at RT for 24 h. After completion of the reaction, the reaction mass was quenched in ice water and stirred for 15 minutes. The obtained solid product was filtered and dried to afford 7.0 g of the desired title product. 1H NMR (300 MHz, DMSO d6): δ 2.26 (s, 6H), 4.36 (t, J=12.3 Hz, 2H), 7.09 (m, 1H), 7.15 (m, 1H), 9.89-9.94 (m, 1H).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US09439890B2 |
| 出典データセット | uspto-grants-2016_09 |
| ORD ID | ord-c521480019fd45eb94312a773d2c8503 |
| 出典メモ | uspto-grants-2016_09 |