Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
HRID 2234283생성일: 2026년 10월 26일
Water → 3-Methoxy-4-[[2-methyl-6-[(2-methyl1,3-thiazol-4-yl)methyl]-3-oxo-2,6,8,10-tetrazabicyclo[5.4.0]undeca-7,9,11-trien-9-yl]amino]-n-(1-methyl-4-piperidyl)benzamide
https://huagongshe.com/reaction/2234283
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Water | HCID 962 | — |
| 반응물 | p-Toluenesulfonic acid | HCID 6101 | — |
| 반응물 | 4-Amino-3-methoxy-n-(1-methylpiperidin-4-yl)benzamide | HCID 11529063 | — |
| 반응물 | 10-Chloro-6-methyl-2-[(2-methyl-1,3-thiazol-4-yl)methyl]-2,6,9,11-tetrazabicyclo[5.4.0]undeca-7,9,11-trien-5-one | HCID 86617577 | — |
| 용매 | Methanol | HCID 887 | — |
| 용매 | 4-Methyl-2-Pentanol | HCID 7910 | — |
| 생성물 | 3-Methoxy-4-[[2-methyl-6-[(2-methyl1,3-thiazol-4-yl)methyl]-3-oxo-2,6,8,10-tetrazabicyclo[5.4.0]undeca-7,9,11-trien-9-yl]amino]-n-(1-methyl-4-piperidyl)benzamide | HCID 68684220 | — |
반응 단계
10-chloro-6-methyl-2-[(2-methyl-1,3-thiazol-4-yl)methyl]-2,6,9,11-tetrazabicyclo[5.4.0]undeca-7,9,11-trien-5-one (Intermediate 101; 58 mg, 0.18 mmol), 4-amino-3-methoxy-N-(1-methyl-4-piperidyl)benzamide (WO06/018220; 49 mg, 0.19 mmol) and p-toluene sulphonic acid (70 mg, 0.37 mmol) were taken up in 4-methyl-2-pentanol (2 mL) and heated to 160° C. in microwave by microwave irradiation for 1 hour. The reaction mixture was dissolved in methanol (5 mL) and water (˜5 mL) and poured directly onto an SCX-3 cartridge (2 g). The cartridge was washed through with methanol (˜30 mL), before elution of products with 2M ammonia in methanol (˜30 mL). Evaporation of the ammoniacal fraction gave an amber film which was purified by reverse phase HPLC to yield the title compound as an off white solid (43 mg, 26%)
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US07709471B2 |
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| 출처 데이터셋 | uspto-grants-2010_05 |
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| ORD ID | ord-ee0da4a715f64827a23937e02a29bf34 |
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| 출처 메모 | uspto-grants-2010_05 |
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