참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Triethylamine | HCID 8471 | — |
| 반응물 | Methanesulfonyl chloride | HCID 31297 | — |
| 반응물 | 4-Amino-N-[2-(diethylamino)ethyl]-2-methoxybenzamide | HCID 77374 | — |
| 반응물 | Sodium Bicarbonate | HCID 516892 | — |
| 용매 | Dichloromethane | HCID 6344 | — |
| 생성물 | HCID 66934940 | HCID 66934940 | 100.1% |
반응 단계
265 mg (1 mmol) of 4-amino-N-(2-diethylamino-ethyl)-2-methoxy-benzamide is introduced into 15 ml of methylene chloride and mixed in succession with 111 mg (1.1 mmol) of triethylamine and 126 mg (1.1 mmol) of methanesulfonic acid chloride. It is stirred for 2 hours at room temperature and then allowed to stand overnight. It is then mixed with 25 ml of saturated sodium bicarbonate solution and shaken out three times with 25 ml each of methylene chloride. The collected organic phase is dried, filtered and concentrated by evaporation. The residue is chromatographed on 10 g of basic silica gel (Isolute flash Si NH2) with a gradient from cyclohexane:ethyl acetate=100:0 to 50:50. 232 mg (52.6% of theory) of N-(2-diethylamino-ethyl)-4-(bismethanesulfonylamino)-2-methoxy-benzamide with a melting point of 144.1° C. is obtained.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US07427390B2 |
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| 출처 데이터셋 | uspto-grants-2008_09 |
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| ORD ID | ord-557ed9ad4750411aa66c4b927f5247f6 |
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| 출처 메모 | uspto-grants-2008_09 |
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