関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | 3-Butenenitrile | HCID 8009 | — |
| 反応物 | 4,4'-Methylenebisbenzenediazonium bis(tetrafluoroborate) | HCID 11732010 | — |
| 触媒 | palladium(II) acetate | HCID 167845 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 生成物 | 4-{4-[4-(3-Cyano-propenyl)-benzyl]-phenyl}-but-3-enenitrile | HCID 57091596 | 61% |
反応手順
A suspension of 4,4′-methanediyl-bis-benzenediazonium tetrafluoroborate (11.9 g, 0.03 mol), prepared according to the method of example 6.1, allyl cyanide (8.05 g; 0.12 mol), and palladium acetate (0.135 g, 0.6 mmol) in 80 ml of ethanol is heated at 40° C. during 22 h. The heterogeneous reaction mixture is poured into 300 ml of water, extracted with ethyl acetate, washed with water, brine, dried over MgSO4, and evaporated. The crude beige product is recrystallized from 130 ml of ethanol, yielding 5.44 g (61%) of 4-{4-[4-(3-cyano-propenyl)-benzyl]-phenyl}-but-3-enenitrile as light beige crystals, melting point 128-130° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US06703182B1 |
|---|
| 出典データセット | uspto-grants-2004_03 |
|---|
| ORD ID | ord-7395024a17624351a2345a5625fb037c |
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| 出典メモ | uspto-grants-2004_03 |
|---|
