関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Tetrahydrofuran | HCID 8028 | — |
| 反応物 | Methoxymethyl-triphenylphosphonium chloride | HCID 2723798 | — |
| 反応物 | HCID 14326170 | HCID 14326170 | — |
| 反応物 | Potassium tert-butoxide | HCID 23665647 | — |
| 溶媒 | Diethyl Ether | HCID 3283 | — |
| 生成物 | Methyl 2-(3-benzyl-2-thienyl)-3-methoxypropenoate | HCID 54504656 | — |
| 生成物 | HCID 67883648 | HCID 67883648 | — |
反応手順
Potassium tert-butoxide (844 mg) was added in one portion to a stirred suspension of (methoxymethyl)triphenylphosphonium chloride (2.86 g) in ether (30 ml). The reaction mixture became red. After 20 minutes, a solution of methyl 2-(3-phenoxymethyl-2-thienyl)-2-oxoacetate (770 mg) in THF (10 ml) was added in one portion and the red colour was discharged. The resulting mixture was stirred at room temperature for 30 minutes then poured into water. The organic and aqueous layers were separated, and the latter was extracted with ether. The combined organic layers were washed with water, dried, concentrated and chromatographed using a 1:1 mixture of ether and petrol as eluent to give (i) the (Z)-isomer of the title compound (230 mg, 27%) as a pale yellow oil, IR (film) 1710, 1625 cm-1, 1H nmr: see Table VII; and (ii) the (E)-isomer of the title compound (80 mg, 9% yield), also a pale yellow oil, IR (film) 1700, 1620 cm-1, 1H nmr: see Table VII.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05258360 |
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| 出典データセット | uspto-grants-1993_11 |
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| ORD ID | ord-f2e71cca8ec84064bb603526505f08e0 |
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| 出典メモ | uspto-grants-1993_11 |
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