関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | p-Toluenesulfonic acid | HCID 6101 | — |
| 反応物 | Methyl 3,4-Dihydroxyphenylacetate | HCID 11008556 | — |
| 反応物 | 1-Chloro-4-[(4-chlorophenyl)-dimethoxymethyl]benzene | HCID 11652307 | — |
| 溶媒 | Toluene | HCID 1140 | — |
| 生成物 | Methyl(2,2-di[4-chlorophenyl]-1,3-benzodioxolan-5-yl)acetate | HCID 54378343 | 37.7% |
反応手順
A mixture of di(4-chlorophenyl)dimethoxymethane (26 g) (see Preparation 13) and methyl (3,4-dihydroxyphenyl)acetate (16 g) (see Preparation 12) in toluene (200 ml) was heated under reflux in a Dean-Stark apparatus for one hour. The reaction was cooled to 60° C. and p-toluenesulphonic acid was added (50 mg). After heating under reflux for 16 hours the solution was cooled, washed with aqueous sodium bicarbonate (100 ml, dried (MgSO4) and evaporated to a brown gum. Flash chromatography (silica, eluant=4:1 hexane/ethyl acetate) gave the title compound as a pale yellow gum (13.7 g). LRMS m/z=415(m)+.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US05922747 |
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| 出典データセット | uspto-grants-1999_07 |
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| ORD ID | ord-864635d2a4624755a8e8f1d9780f6c28 |
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| 出典メモ | uspto-grants-1999_07 |
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