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Triethylamine → HCID 59253981、化合物
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | Benzyloxyacetyl chloride | HCID 177085 | — |
| 反応物 | 6-(4-Aminophenoxy)-hexanoic acid methyl ester | HCID 14650296 | — |
| 溶媒 | Acetone | HCID 180 | — |
| 生成物 | HCID 59253981 | HCID 59253981 | 22.2% |
反応手順
To a mixture of 6-(4-aminophenoxy)-hexanoic acid methyl ester 17 (25 g, 105 mmol) and triethylamine (21.4 g, 211.6 mmol) in acetone (200 ml) at 0° C. was added dropwise benzyloxy acetyl chloride (25 g, 135.5 mmol) followed by stirring at room temp. for 12 hrs. The solids were filtered off, acetone distilled off and water (100 ml) added. Crude 53 was extracted into chloroform, washed with 5% sodium bicarbonate solution (2×100 ml), then water (100 ml), dried over sodium sulphate and distilled. Crude 53 was purified by column chromatography on silica gel using benzene as eluant to get pure 53 (9 g, 22.2%), an off-white powder with a m.p. between 46-49° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07772352B2 |
| 出典データセット | uspto-grants-2010_08 |
| ORD ID | ord-b6e58a072fec47b98761066fa012a2fa |
| 出典メモ | uspto-grants-2010_08 |