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Water → Methyl 4-[3-(2-chloro-ethoxy)-propionyl-amino]-3-methyl-benzoate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | Methyl 4-amino-3-methylbenzoate | HCID 2736799 | — |
| 反応物 | 3-(2-Chloroethoxy)propanoyl chloride | HCID 86069372 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | Methyl 4-[3-(2-chloro-ethoxy)-propionyl-amino]-3-methyl-benzoate | HCID 67048278 | — |
反応手順
1.70 g (10.3 mmol) methyl 4-amino-3-methyl-benzoate in 10 ml THF are combined with 2.84 ml (20.6 mmol) triethylamine and stirred for 20 minutes at ambient temperature. Then a solution of 1.78 g (10.4 mmol) 3-(2-chloro-ethoxy)-propionic acid-chloride in 25 ml THF is added dropwise and the mixture is stirred for a further 2.5 hours at ambient temperature. Then water is added and the mixture is extracted with ethyl acetate. The combined organic phases are dried over sodium sulphate and evaporated down completely i. vac. The residue is purified by chromatography on silica gel (eluting gradient: petroleum ether/ethyl acetate=7:3->6:4).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08791103B2 |
| 出典データセット | uspto-grants-2014_07 |
| ORD ID | ord-8e63cca2dad34161a4577676e874426d |
| 出典メモ | uspto-grants-2014_07 |