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Calcium Hydroxide → 6-Methylphthalide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Calcium Hydroxide | HCID 6093208 | — |
| 反応物 | 6-(Bromomethyl)isobenzofuran-1(3H)-one | HCID 15190685 | — |
| 反応物 | HCID 178418361 | HCID 178418361 | — |
| 触媒 | Palladium | HCID 23938 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 溶媒 | 1,4-Dioxane | HCID 31275 | — |
| 生成物 | 6-Methylphthalide | HCID 638756 | 96% |
反応手順
A total of 107 g (472 mmol) of 6-bromomethylphthalide was dissolved in 50 mL of methanol (dioxane was also used in different experiment). The solution was added to a parr bottle with 40 g (540 mmol) of calcium hydroxide and 2 g of 10% Pd/C. The suspension was hydrogenated at 40 psi until no more hydrogen uptake was recorded. All solids were filtered and filtrate was concentrated to a total of 67 g of brown solid in 96% yield. 1H NMR (CDCl3) (300 MHz) δ 2.53 (s, 3H), 5.30 (s, 2H), 7.49 (s 1H), 7.54 (d, 3JHCCH=7.9 Hz, 1H), 7.47 (d, 3JHCCH=7.9 Hz, 1H)
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08431721B2 |
| 出典データセット | uspto-grants-2013_04 |
| ORD ID | ord-b7f7538792b344a79181375727b0566d |
| 出典メモ | uspto-grants-2013_04 |