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Ethyl 2-methylacetoacetate → 5-Ethyloxycarbonyl-5-methyl-6-oxo-1-heptanesulfonic acid
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Ethyl 2-methylacetoacetate | HCID 701 | — |
| 反応物 | 1,4-Butane sultone | HCID 15411 | — |
| 反応物 | HCID 178418922 | HCID 178418922 | — |
| 溶媒 | tert-Butanol | HCID 6386 | — |
| 生成物 | 5-Ethyloxycarbonyl-5-methyl-6-oxo-1-heptanesulfonic acid | HCID 58084006 | 75% |
反応手順
0.35 ml (3.47 mmol) of 1,4-butane sultone were added to a mixture of 0.49 ml (3.47 mmol) ethyl 2-methylacetoacetate and 513 mg (4.2 mmol) of tert-BuOK in 12 ml tert-butanol and refluxed for 15 hours. The formed precipitate was filtered and washed with hexane to yield 730 mg of 5-ethyloxycarbonyl-5-methyl-6-oxo-1-heptanesulfonic acid. δH (200 MHz, DMSO-d6): 4.12 (2H, q, 7.1, 14.2 Hz, OCH2), 3.97 (2H, t, 5.8 Hz, CH2SO3H), 2.10 (3H, s, COCH3), 1.78-1.41 (4H, m, CH2), 1.24-1.01 (2H, m, CH2), 1.22 (3H, s, CCH3), 1.17 (3H, t, 7.3 Hz, CH2CH3).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US09110069B2 |
| 出典データセット | uspto-grants-2015_08 |
| ORD ID | ord-2e1a968278cf48e39fc4abe11e9aaf6f |
| 出典メモ | uspto-grants-2015_08 |