참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Sodium peroxide | HCID 14803 | — |
| 반응물 | 1-t-Butylazo-1-chlorocyclohexane | HCID 23344784 | — |
| 용매 | Methanol | HCID 887 | — |
| 생성물 | HCID 20367916 | HCID 20367916 | 100.1% |
반응 단계
To a solution of 0.78 grams (.01 moles) of sodium peroxide in 30 ml. of methanol, cooled to 10° C in a 50 ml. erlenmeyer flask immersed in a cold water bath was added 4.3 grams (.0213 moles) of 1-t-butylazo-1-chlorocyclo-hexane dropwise and with rapid stirring holding the temperature at 10°-15° C. After the addition was complete, the reaction was stirred for 1 hour at 5° C. It was then poured in 250 ml. of ice cold water and the product extracted with pentane. The pentane layer was separated, washed with saturated (NH4)2SO4, water, saturated NaHCO3, water, dried, filtered and the pentane evaporated under reduced pressure to give 3.67 grams (85% yield) of crude di[1-(t-butylazo)cyclohexyl] peroxide. The infrared spectrum indicated the product was contaminated to a small extent by 1-t-butylazo-1-methoxy-cyclohexane which resulted from the chloro compound reacting to a small extent with the methanol solvent.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US04075199 |
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| 출처 데이터셋 | uspto-grants-1978_02 |
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| ORD ID | ord-4648701b3c0c48e7a5cd47961c5580c5 |
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| 출처 메모 | uspto-grants-1978_02 |
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