関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Diisopropylamine | HCID 7912 | — |
| 反応物 | Cyclohexane | HCID 8078 | — |
| 反応物 | 3-Methyl-2-butenenitrile | HCID 94301 | — |
| 反応物 | 1-(Isopropylsulfonyl)-4-methylbenzene | HCID 816792 | — |
| 反応物 | Monosodium phosphate | HCID 23672064 | — |
| 反応物 | Butyllithium | HCID 178418339 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | 4-p-Tolylsulfonyl-4,3,3,-trimethyl-pentanenitrile | HCID 12833028 | — |
反応手順
3.81 ml of a cyclohexane solution of 1.75M of butyllithium were added at -30° to -40° C. to a mixture of 1.05 ml of diisopropylamine and 4 ml of tetrahydrofuran and the mixture was stirred for 10 minutes and was then cooled to -60° to -70° C. Then 1.22 g of p-tolyl isopropylsulfone were added to the mixture which after 15 minutes of contact was poured over 10 minutes under an inert atmosphere into a solution of 0.5 g of dimethylacrylonitrile and 4 ml of tetrahydrofuran at -60° to -70° C. The mixture was stirred for 30 minutes at -60° to -70° C. and was then poured into an aqueous saturated monosodium phosphate solution. The mixture was extracted with benzene and the organic phase was dried and evaporated to dryness. The residue was crystallized from isopropyl ether to obtain 0.740 g of 4-p-tolylsulfonyl-4,3,3,-trimethyl-pentanenitrile melting at 126° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US04401601 |
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| 出典データセット | uspto-grants-1983_08 |
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| ORD ID | ord-65212fa3874a4fbfb05ef8243326a26e |
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| 出典メモ | uspto-grants-1983_08 |
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