참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Dimethylformamide | HCID 6228 | — |
| 반응물 | Benzo(b)thiophene-2-carboxylic acid | HCID 95864 | — |
| 반응물 | Sodium Bicarbonate | HCID 516892 | — |
| 반응물 | 6,6-Difluoro-5-methyl-5-hexenyl methanesulfonate | HCID 23020371 | — |
| 용매 | Water | HCID 962 | — |
| 생성물 | 6,6-Difluoro-5-methyl-5-hexenyl benzo[b]thiophene-2-carboxylate | HCID 69181690 | 81% |
반응 단계
To 40 ml of N,N-dimethylformamide were dissolved 5.00 g (22 mmol) of 6,6-difluoro-5-methyl-5-hexenyl methanesulfonate and 4.30 g (24 mmol) of benzo[b]thiophene-2-carboxylicacid, followed by the addition of 6.00 g (71 mmol) of sodium hydrogencarbonate and stirring at 100° C. for 3 hours. The reaction liquid was then poured in water and extracted with diethyl ether. The organic layer was washed with water and a saturated saline solution in this order, followed by drying over anhydrous magnesium sulfate and concentration under reduced pressure. The residue was purified with silica gel column chromatography (diisopropyl ether:hexane=1:7) to obtain 5.50 g (yield: 81%) of 6,6-difluoro-5-methyl-5-hexenyl benzo[b]thiophene-2-carboxylate.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US07273878B2 |
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| 출처 데이터셋 | uspto-grants-2007_09 |
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| ORD ID | ord-9db6e71ddd914462931406307e242912 |
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| 출처 메모 | uspto-grants-2007_09 |
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