참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Dimethyl Sulfoxide | HCID 679 | — |
| 반응물 | Methylamine | HCID 6329 | — |
| 반응물 | 3,5-Dinitropyridine-2,6-diamine | HCID 542959 | — |
| 용매 | Methanol | HCID 887 | — |
| 용매 | Dimethylacetamide | HCID 31374 | — |
| 생성물 | 2,6-Di(methylamino)-3,5-dinitropyridine | HCID 21554890 | — |
반응 단계
To a solution of 2,6-diamino-3,5-dinitropyridine (25.0 g, 0.125 mole) and 225 ml dimethylsulfoxide in a 500 ml Parr bottle was added a solution of methylamine (20 g, 0.65 mole) in 75 ml N,N-dimethylacetamide (DMAc). The reaction was shaken for 4 hours at ambient temperatures and then heated 20 hours at 70°C. Upon cooling, the heterogeneous mixture was diluted with 100 ml methanol, filtered, washed with 200 ml DMAc-methanol (lv/lv), twice with methanol and dried. 2,6-Di(methylamino)-3,5-dinitropyridine, m.p. 323°-325°C (dec.) was obtained as a golden yellow solid (25.0 g, 93% yield). This product, unlike 2,6-diamino-3,5-dinitropyridine, is essentially insoluble in dimethylsulfoxide and 85% H3PO4. Anal. Calcd. for C7H9N5O4 : C, 37.0; H, 4.0; N, 30.8. Found: C, 37.2; H, 3.8; N, 31.0.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US03943125 |
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| 출처 데이터셋 | uspto-grants-1976_03 |
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| ORD ID | ord-c53048a57f57486b8ed6b1a221694a0b |
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| 출처 메모 | uspto-grants-1976_03 |
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