참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Carbon Disulfide | HCID 6348 | — |
| 반응물 | Beta-Nitrostyrene | HCID 7626 | — |
| 반응물 | Piperidinium 1-piperidinecarbodithioate | HCID 2820349 | — |
| 용매 | Methanol | HCID 887 | — |
| 생성물 | alpha-(Nitromethyl)benzyl 1-piperidinecarbodithioate | HCID 11266906 | — |
반응 단계
β-Nitrostyrene (14.9 grams, 0.10 mole) was added in portions to a stirred mixture of piperidinium 1-piperidinecarbodithioate (24.6 grams, 0.10 mole), and carbon disulfide (7.6 grams, 0.10 mole) in methanol (200 ml.). During the addition, the reaction temperature was 25° C.-29° C. After the addition of β-nitrostyrene, the reaction mixture was cooled to 8° C., and the precipitated product was filtered off, washed with water, and dried in air. The yield of product melting at 85° C.-87° C. (prior sintering) was 29.0 grams (93%). Repeated recrystallizations without heating from methylene chloride-hexane and methylene chloride-methanol solutions gave pure α-(nitromethyl)benzyl 1-piperidinecarbodithioate melting at 86° C.-90.5° C. (prior sintering).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US04011230 |
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| 출처 데이터셋 | uspto-grants-1977_03 |
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| ORD ID | ord-ae882f0193e946c4bdea7fcb06b2bf74 |
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| 출처 메모 | uspto-grants-1977_03 |
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