関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | 2-Methyl-2-butenal | HCID 10336 | — |
| 反応物 | Myrcene | HCID 31253 | — |
| 反応物 | Ethyl aluminium dichloride | HCID 16686341 | — |
| 触媒 | Ethyl aluminium dichloride | HCID 16686341 | — |
| 溶媒 | Benzene | HCID 241 | — |
| 生成物 | 1,6-Dimethyl-4-(4-methyl-3-pentenyl)-3-cyclohexene-1-carboxaldehyde | HCID 19861574 | 44.7% |
反応手順
A 3-neck reaction vessel is charged with 100 ml benzene and 50 grams of 25% ethyl aluminum dichloride in benzene. A solution containing 320 grams myrcene (85% pure), 170 grams 2-methyl-2-butenal, and 200 ml benzene is fed in at 40°-50° C. over a 1 hour period. The temperature is then raised to 60° C. and held there for 1/2 hour. An additional 10 grams ethyl aluminum dichloride solution mixed with 20 ml benzene is added and heating is continued for an additional 1/2 hour. The mixture is then cooled, water is added and the layers are separated. The organic layer is washed with water and distilled without fractionation to free the material of residue. Redistillation through an 18" Goodlow packed column provides 199 grams of 1,6-dimethyl-4-(4-methyl-3-pentenyl)-3-cyclohexene-1-carboxaldehyde (b.p. 105° C., 0.9 mm).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | USRE032721 |
|---|
| 出典データセット | uspto-grants-1988_07 |
|---|
| ORD ID | ord-de6f272f5e184021a35216daf0c2786d |
|---|
| 出典メモ | uspto-grants-1988_07 |
|---|