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Methanol → Methyl [4-(4-hydroxy-3,5-diiodophenoxy)-3,5-diiodophenyl]acetate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Methanol | HCID 887 | — |
| 反応物 | Water | HCID 962 | — |
| 反応物 | Thionyl Chloride | HCID 24386 | — |
| 反応物 | Tetraiodothyroacetic acid | HCID 65552 | — |
| 生成物 | Methyl [4-(4-hydroxy-3,5-diiodophenoxy)-3,5-diiodophenyl]acetate | HCID 52919069 | — |
反応手順
[4-(4-Hydroxy-3,5-diiodophenoxy)-3,5-diiodophenyl]acetic acid (5.0 g, 6.7 mmol, 1.0 equiv.) was dissolved in 200 mL of dried MeOH. Then thionyl chloride (485 μL, 6.7 mmol, 1.0 equiv.) was added drop wise. The reaction was set to reflux for 2 days. Water was then added to the reaction medium (200 mL) and then the solution was concentrated. The precipitated product was collected by filtration and then the aqueous phase analyzed by TLC but showed to contain no product. The solid was then re-crystallized in EtOH, filtered and washed with cold EtOH before being dried under vacuum.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08859539B2 |
| 出典データセット | uspto-grants-2014_10 |
| ORD ID | ord-331be737d9e84e4a938b81d1b0f4770f |
| 出典メモ | uspto-grants-2014_10 |