関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Formaldehyde | HCID 712 | — |
| 反応物 | Methanol | HCID 887 | — |
| 反応物 | 2-Hydroxy-5-methylacetophenone | HCID 15068 | — |
| 生成物 | 2'-Hydroxy-5'-methyl-3'-methoxymethylacetophenone | HCID 13229232 | — |
反応手順
A mixture of 2′-hydroxy-5′-methylacetophenone (1.0 g, 6.7 mmol) was treated with paraformaldehyde (0.18 g) and conc. hydrochloric acid (5 ml) and the mixture heated at 60° C. overnight. Upon cooling the mixture was extracted with toluene (3×30 ml) and the combined extracts were dried (Na2SO4) and the solvent removed to yield a yellow oil. The oil was treated with methanol (30 ml) and heated to reflux for 1 h. Upon cooling, the solution was evaporated to near dryness, and the residue chromatographed on a silica column, eluting with 0-10% ethyl acetate in petroleum ether. The purified product was obtained as an white powder (0.76 g)
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07598377B2 |
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| 出典データセット | uspto-grants-2009_10 |
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| ORD ID | ord-a4f47ab135884ac1ab6ca877253c4acd |
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| 出典メモ | uspto-grants-2009_10 |
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