참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Boron trifluoride | HCID 6356 | — |
| 반응물 | 1,4-Dioxane | HCID 31275 | — |
| 반응물 | 2(3H)-Benzothiazolone, 6-amino- | HCID 6453329 | — |
| 반응물 | Sodium Nitrite | HCID 23668193 | — |
| 촉매 | palladium(II) acetate | HCID 167845 | — |
| 용매 | Water | HCID 962 | — |
| 용매 | Diethyl Ether | HCID 3283 | — |
| 용매 | Tetrafluoroboric acid | HCID 28118 | — |
| 생성물 | 6-(2-Phenylethenyl)-1,3-benzothiazol-2(3H)-one | HCID 69798817 | — |
반응 단계
The compound obtained in Step B (1 g) is dissolved in HBF4 (10 ml) and the mixture is cooled to 0° C. 0.44 g of NaNO2 previously dissolved in water is then added and the reaction is stirred at 0° C. for 1 hour. The resulting precipitate is filtered off and washed with ether, ground with BF3 (4.5 mmol) and palladium acetate (0.2 mmol), and then placed under a nitrogen atmosphere before the addition of 15.1 ml of anhydrous dioxane. The reaction mixture is stirred for 5 hours at ambient temperature and then hydrolysis is carried out with 50 ml of water and extraction is carried out twice with 30 ml ether each time. The organic phase is dried over MgSO4 and then evaporated under reduced pressure. The resulting precipitate is washed with isopropyl ether and recrystallised from methanol.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US06919362B2 |
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| 출처 데이터셋 | uspto-grants-2005_07 |
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| ORD ID | ord-3d90499e44dc45a49dd83d8f19846c8b |
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| 출처 메모 | uspto-grants-2005_07 |
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