関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 1,2-Dichlorobenzene | HCID 7239 | — |
| 反応物 | Methyl 4-(allyloxy)benzoate | HCID 4645407 | — |
| 生成物 | Methyl 3-allyl-4-hydroxybenzoate | HCID 939882 | 91% |
反応手順
A solution of 15.05 g (78.3 mmol) of the product of Step A in 25 mL of 1,2-dichlorobenzene was magnetically stirred and refluxed (183° C.) under an argon atmosphere for 18 hours. At this point, the reaction mixture was cooled to room temperature and applied to a 6 cm diameter by 18 cm silica gel flash chromatography column and eluted with 25% ethyl acetate-hexane to separate the 1,2-dichlorobenzene, then with 40% ethyl acetate-hexane to elute the product. The product fractions were concentrated in vacuo and the residual oil was crystallized from hexane to afford 13.70 g (91%) of the title compound.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US05264439 |
|---|
| 出典データセット | uspto-grants-1993_11 |
|---|
| ORD ID | ord-6d5945decc894a7db381087089464d5f |
|---|
| 出典メモ | uspto-grants-1993_11 |
|---|