참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Acetone Cyanohydrin | HCID 6406 | — |
| 반응물 | Triethylamine | HCID 8471 | — |
| 반응물 | Dimedone | HCID 31358 | — |
| 반응물 | 4-(Methanesulfonyl)-2-nitrobenzoyl chloride | HCID 14800186 | — |
| 용매 | Dichloromethane | HCID 6344 | — |
| 생성물 | 2-(4-Methylsulphonyl-2-nitrobenzoyl)-5,5-dimethylcyclohexane-1,3-dione | HCID 19937139 | 48.8% |
반응 단계
A solution of 4-methylsulphonyl-2-nitrobenzoyl chloride (9.62 g) in dry dichloromethane (50 ml) was added to a stirred solution of triethylamine (5.6 ml) and 5,5-dimethylcyclohexane-1,3-dione (5 g) in dry dichloromethane (70 ml) during 30 minutes and the reaction mixture stirred at ambient temperature for 4 hours. Triethylamine (15.3 ml) and acetone cyanohydrin (0.5 ml) were added successively and the reaction mixture stirred at ambient temperature for 18 hours. The reaction mixture was washed successively with 2N hydrochloric acid (2×50 ml) and water (2×50 ml), dried over magnesium sulphate and evaporated under reduced pressure to give a yellow glass which was recrystallised from methanol (20 ml) to give 2-(4-methylsulphonyl-2-nitrobenzoyl)-5,5-dimethylcyclohexane-1,3-dione (6.4 g), m.p. 156.5°-158° C., as a yellow crystalline solid.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US05416061 |
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| 출처 데이터셋 | uspto-grants-1995_05 |
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| ORD ID | ord-d58fcbdd740644d9af498b7e9b6eb406 |
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| 출처 메모 | uspto-grants-1995_05 |
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