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Triclosan → 5-Chloro-2-(2,4-dichlorophenoxy)phenyl 4-carboxy-3-methylbutyrate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Triclosan | HCID 5564 | — |
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | 3-Methylglutaric anhydride | HCID 77828 | — |
| 溶媒 | Diethyl Ether | HCID 3283 | — |
| 生成物 | 5-Chloro-2-(2,4-dichlorophenoxy)phenyl 4-carboxy-3-methylbutyrate | HCID 23322896 | 23% |
反応手順
A mixture of triclosan (22.3 g.), 3-methylglutaric anhydride (15.0 g.) and triethylamine (15 ml.) in ether (250 ml.) was stirred for 20 hours, and then washed first with 2M hydrochloric acid (50 ml.) and then with water (3×150 ml.). The ether phase was dried (MgSO4) and evaporated. A portion (20 g.) of the residual oil was purified by chromatography on silica gel using methylene chloride as eluant to give (D) as a colourless oil (7.4 g.) ; NMR (CDCl3): 0.8-1.3 (3H,d, CH3), 2.1-2.8 (5H,m,CH2CO+CH3CH), 6.7-7.6 (6H, m, aromatic H), 11.25 (1H,s, CO2H)ppm.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04587262 |
| 出典データセット | uspto-grants-1986_05 |
| ORD ID | ord-9c22268e69f445f58f3de5e07ed5e4a6 |
| 出典メモ | uspto-grants-1986_05 |