참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Sodium hydride | HCID 24758 | — |
| 반응물 | Methane, sulfinylbis-, ion(1-), sodium | HCID 10154010 | — |
| 반응물 | ethyl 5-(2-aminophenylamino)-1-methyl-1H-pyrazole-4-carboxylate | HCID 57555331 | — |
| 용매 | Dimethyl Sulfoxide | HCID 679 | — |
| 생성물 | 1-methyl-5,10-dihydrobenzo[b]pyrazolo[3,4-e][1,4]diazepin-4(1H)-one | HCID 135736034 | 40% |
반응 단계
Sodium (methylsulphinyl)methanide (29.7 mmol) was pre-pared from sodium hydride (60% dispersion in oil, 1.19 g, 29.7 mmol) and anhydrous dimethyl sulphoxide (7 ml) by heating at 65° C. until a solution was observed. To this was added a solution of 5-(2-amino-phenylamino)-1-methyl-1H-pyrazole-4-carboxylic acid ethyl ester from Example E11.2 (3.63 g, 16.9 mmol) in anhydrous dimethyl sulphoxide (10 ml), and stirring continued at 65° C. for 2.5 h. The mixture was poured into ice (100 ml), and the resulting solid collected and purified by recrystallisation from methanol/EtOAc/60-80 pet ether to yield the title compound (1.46 g, 40%).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US08202858B2 |
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| 출처 데이터셋 | uspto-grants-2012_06 |
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| ORD ID | ord-3e583a73eb614ed2a392213d44410395 |
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| 출처 메모 | uspto-grants-2012_06 |
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