関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Methane, dichloromethoxy- | HCID 21004 | — |
| 反応物 | N-Ethyloxindole | HCID 66135 | — |
| 触媒 | Titanium Tetrachloride | HCID 24193 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 1-Ethyl-5-formyloxindole | HCID 13770522 | 76% |
反応手順
To a solution of 32.2 g. (0.2 mole) of 1-ethyloxindole in 200 ml. of methylene chloride was added 44 ml. (0.4 mole) of titanium tetrachloride followed by 22.6 ml. (0.25 mole) of dichloromethyl methyl ether. The reaction was stirred for 10.5 days at 25° C. followed by the addition of additional titanium tetrachloride and dichloromethyl methyl ether every 48 hours. The reaction was poured onto 1 l. of ice and water and extracted with methylene chloride. Concentration of the dried extract gave the crude product which was recrystallized from diethyl ether, 28.6 g. (76% yield), m.p. 126°-127° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US04644005 |
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| 出典データセット | uspto-grants-1987_02 |
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| ORD ID | ord-05ae04dbe4754f18a2fe9e83b1959cf3 |
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| 出典メモ | uspto-grants-1987_02 |
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