참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Hydrochloric Acid | HCID 313 | — |
| 반응물 | Sodium hydride | HCID 24758 | — |
| 반응물 | Ethyl 2-thenoate | HCID 76052 | — |
| 반응물 | 1-(4-(Trifluoromethoxy)phenyl)ethan-1-one | HCID 522821 | — |
| 용매 | Water | HCID 962 | — |
| 용매 | Tetrahydrofuran | HCID 8028 | — |
| 생성물 | 1-(2-Thienyl)-3-(4-trifluoromethoxyphenyl)-1,3-propanedione | HCID 18175613 | 99.4% |
반응 단계
4-Trifluoromethoxyacetophenone (4.1 g, 20 mM) and ethyl 2-thiophenecarboxylate (3.1 g, 20 mM) were placed in a 300 ml eggplant type flask, and 100 ml of dehydrated tetrahydrofuran was added thereto. After this mixture was stirred at room temperature, a 60% oil suspension of sodium hydride (1.1 g, 26 mM) was slowly added thereto. Thereafter, the resulting mixture was heated under reflux for 6 hours and allowed to cool to room temperature. After 100 ml of water was added to the reaction mixture under cooling with ice, the reaction mixture was adjusted to pH 1.0 with a concentrated aqueous solution of hydrochloric acid and then extracted with 100 ml of ethyl acetate. The organic layer was washed with a saturated aqueous solution of sodium chloride and dried over anhydrous sodium sulfate. Thereafter, the solvent was distilled off under reduced pressure to obtain 6.2 g of 1-(2-thienyl)-3-(4-trifluoromethoxyphenyl)-1,3-propanedione in an almost quantitative yield.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US06605730B2 |
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| 출처 데이터셋 | uspto-grants-2003_08 |
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| ORD ID | ord-84aaee33eb444d69b76e6f4e59f912b5 |
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| 출처 메모 | uspto-grants-2003_08 |
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