참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Guanidine | HCID 3520 | — |
| 반응물 | Guanidine Hydrochloride | HCID 5742 | — |
| 반응물 | Sodium Methoxide | HCID 10942334 | — |
| 반응물 | 3-(7,8-Dimethoxy-2H-1-benzopyran-5-yl)-2-methoxymethylpropenenitrile | HCID 54373447 | — |
| 용매 | Methanol | HCID 887 | — |
| 생성물 | 2,4-diamino-5-(7,8-dimethoxy-2H-1-benzopyran-5-ylmethyl)pyrimidine | HCID 12849772 | 42.8% |
반응 단계
Guanidine hydrochloride (11.46 g, 0.12 mole) in methanol (25 mL) was added to sodium methoxide (6.55 g, 0.12 mole) in methanol (40 mL) and the resultant sodium chloride was filtered and washed with methanol (10 mL). The guanidine solution was added to 3-(7,8-dimethoxy-2H-1-benzopyran-5-yl)-2-methoxymethylpropenenitrile (11.5 g, 0.04 mole) and the mixture heated at reflux for 2 hr. Cooling the mixture at 3° C. provided 5.38 g of yellow solid in two crops. HPLC assayed yield of 28.6%. A sample recrystallized from alcohol/water gave mp 232°-4° C.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US04761475 |
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| 출처 데이터셋 | uspto-grants-1988_08 |
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| ORD ID | ord-817e59b075864a43ba1165743bca3c56 |
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| 출처 메모 | uspto-grants-1988_08 |
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