参与物
| 角色 | 名称 | HCID | 投料 |
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| 反应物 | 过氧化钠 | HCID 14803 | — |
| 反应物 | 1-t-Butylazo-1-chlorocyclohexane | HCID 23344784 | — |
| 溶剂 | (5BETA,17BETA)-17-羟基-17-(甲基-D3)-2'H-雄甾-2-烯并[3,2-C]吡唑-5'(1'H)-酮 | HCID 887 | — |
| 产物 | HCID 20367916 | HCID 20367916 | 100.1% |
反应步骤
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.
来源与证据
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 专利号 | US04075199 |
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| 来源数据集 | uspto-grants-1978_02 |
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| ORD ID | ord-4648701b3c0c48e7a5cd47961c5580c5 |
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| 来源说明 | uspto-grants-1978_02 |
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