참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Hydrochloric Acid | HCID 313 | — |
| 반응물 | Triethylamine | HCID 8471 | — |
| 반응물 | 2-Aminobenzophenone | HCID 76080 | — |
| 반응물 | Tert-Butyl hypochlorite | HCID 521297 | — |
| 반응물 | Ethyl 2-(methylthio)propionate | HCID 3016224 | — |
| 용매 | Dichloromethane | HCID 6344 | — |
| 생성물 | 7-Benzoyl-3-methyl-3-(methylsulfanyl)-1,3-dihydro-2H-indol-2-one | HCID 12909816 | — |
반응 단계
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.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US04045576 |
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| 출처 데이터셋 | uspto-grants-1977_08 |
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| ORD ID | ord-499c401190c3414e9bb4ce3a69c33369 |
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| 출처 메모 | uspto-grants-1977_08 |
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