참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Pyridine | HCID 1049 | — |
| 반응물 | Methanesulfonyl chloride | HCID 31297 | — |
| 반응물 | 2,5-Diamino-benzenesulfonamide methanesulfonate | HCID 25164641 | — |
| 용매 | Acetonitrile | HCID 6342 | — |
| 생성물 | 2-Amino-5-[(methylsulfonyl)amino]benzenesulfonamide | HCID 24950657 | 86.3% |
반응 단계
2,5-Diamino-benzenesulfonamide methanesulfonate (1.80 kg, 6.35 mol) was suspended in acetonitrile (24 L). Pyridine (1.55 L, 19.1 mol) was added, followed by the careful slow addition of methanesulfonyl chloride (517 mL, 6.68 mol). After stirring at 23° C. for 20 h, the mixture was partially concentrated in vacuo at 55° C. Water (18 L) was added to the concentrate, and the resulting suspension was stirred at 23° C. for 2 h. The solid was filtered and was then washed with water (4 L) and air dried on the filter. The solid was suspended in absolute ethanol (9 L), stirred at 23° C. for 9 h, and was then filtered. The solid was washed with absolute ethanol (2×2 L), and was then further dried in vacuo at 50° C. to afford the desired product, 2-amino-5-methanesulfonylamino-benzenesulfonamide (1.45 kg, 5.48 mol, 86%), as a purple solid.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US08101800B2 |
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| 출처 데이터셋 | uspto-grants-2012_01 |
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| ORD ID | ord-e211364c44764adc8de3a06420094d63 |
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| 출처 메모 | uspto-grants-2012_01 |
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