関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | 2-Aminobenzophenone | HCID 76080 | — |
| 反応物 | Tert-Butyl hypochlorite | HCID 521297 | — |
| 反応物 | Ethyl 2-(methylthio)propionate | HCID 3016224 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 7-Benzoyl-3-methyl-3-(methylsulfanyl)-1,3-dihydro-2H-indol-2-one | HCID 12909816 | — |
反応手順
A stirred solution of 3.94 g. (0.02 mole) of 2-aminobenzophenone in methylene chloride at -65° C. was treated with 2.16 g. (0.02 mole) of t-butylhypochlorite. After 15 min. 2.96 g. ethyl α-(methylthio)propionate was added dropwise and stirring continued for 1 hr. At the end of this time 2.02 g. of triethylamine (0.02 mole) was added dropwise and the reaction solution was allowed to warm to room temperature. This was followed by treatment with 1N hydrochloric acid and stirred for 15 min. The methylene chloride solution was then separated and stripped under vacuum. The yellow oil residue was triturated with isopropyl ether and 3 g. of a yellow solid was filtered off (51%). Recrystallization from absolute ethanol gave a cream color solid, m.p. 135°-137° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US04045576 |
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| 出典データセット | uspto-grants-1977_08 |
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| ORD ID | ord-499c401190c3414e9bb4ce3a69c33369 |
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| 出典メモ | uspto-grants-1977_08 |
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