참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | 9-Acetyl-9H-carbazole | HCID 95837 | — |
| 반응물 | 3-(Aminosulfonyl)-4-chlorobenzoyl chloride | HCID 3017979 | — |
| 반응물 | Aluminum(III) Chloride | HCID 6451240 | — |
| 용매 | Dichloromethane | HCID 6344 | — |
| 생성물 | HCID 66850646 | HCID 66850646 | — |
반응 단계
To a solution of 1 g of 1-carbazol-9-yl-ethanone and 2.43 g of 4-chloro-3-sulfamoyl-benzoyl chloride in methylene chloride (20 mL) is added 2.55 g of aluminum chloride. The mixture is stirred at 50° C. overnight. The solution is then cooled at −78° C., quenched with a 6 N HCl solution and allowed to warm up to room temperature. Methylene chloride is added to dissolve the precipitate and the solution is extracted, washed with a saturated sodium chloride solution, dried over sodium sulfate, filtered and concentrated. The residue is loaded on Celite and purified by silica gel chromatography (1:1 hexanes/ethyl acetate) to afford 5-(9-acetyl-9H-carbazole-2-carbonyl)-2-chloro-benzenesulfonamide as yellow foam. MS (m/z): 427 (M+1). HPLC Reverse Phase (Nucleosil 100-5 C18, gradient 10→100% CH3CN in 5 min) room temperature=5.35 minutes.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US08975439B2 |
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| 출처 데이터셋 | uspto-grants-2015_03 |
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| ORD ID | ord-b058d22797e14c7aaa7d8336d8ca5540 |
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| 출처 메모 | uspto-grants-2015_03 |
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