関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Sodium thiocyanate | HCID 516871 | — |
| 反応物 | (E)-1-tert-Butyl-2-(2-chloro-4-methylpentan-2-yl)diazene | HCID 23344796 | — |
| 溶媒 | Isopropanol | HCID 3776 | — |
| 生成物 | 63805-96-9 | HCID 21431168 | — |
反応手順
To a stirred solution of 26.1 grams (0.3 moles) of sodium thiocyanate in 150 ml of 75% aqueous isopropanol in a 500 ml erlenmeyer flask, cooled to 5° C., was added 61.2 grams (0.3 moles) of 2-t-butylazo- 2-chloro-4-methylpentane holding the reaction temperature at 10°-20° C. After the addition was complete, the reaction mixture was stirred an additional two hours at 30° C., poured into 300 ml water and the product extracted with 200 ml pentane. The pentane extract was washed with water, 10% NaHCO3 solution, dried over anhydrous sodium sulfate, filtered and the pentane evaporated under reduced pressure to leave 55.7 grams (80% crude yield) of a yellow liquid. The product had a strong broad band at 1980- 2080 cm-1 in its infrared spectrum which is indicative of the isothiocyano band.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US04028344 |
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| 出典データセット | uspto-grants-1977_06 |
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| ORD ID | ord-d5c486a9375c4a3fb176a4ef4a256d07 |
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| 出典メモ | uspto-grants-1977_06 |
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