関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Sodium Bicarbonate | HCID 516892 | — |
| 反応物 | Boron tribromide methyl sulfide | HCID 10946916 | — |
| 反応物 | 6-hydroxy-1-oxo-3-phenyl-1H-indene-2-carboxylic acid methyl ester | HCID 68700263 | — |
| 溶媒 | 1,1-Dichloroethane | HCID 6365 | — |
| 生成物 | 6-hydroxy-1-oxo-3-phenyl-1H-indene-2-carboxylic acid | HCID 68698982 | 48.6% |
反応手順
6-Hydroxy-1-oxo-3-phenyl-1H-indene-2-carboxylic acid methyl ester (2.6 g, 9.28 mmol) obtained in Step 1 was dissolved in dichloroethane, and boron tribromide methyl sulfide (6.0 mL, 27.84 mmol) was added thereto. The mixture was refluxed for 2 hrs at 90° C., cooled in an ice bath, neutralized using sodium bicarbonate, and adjusted to pH 2 using 6N hydrochloric acid. The resulting mixture washed successively with dichloromethane and water. The organic layer was separated, dried over anhydrous MgSO4, concentrated under a reduced pressure and recrystallized to obtain 1.2 g of the titled compound (yield: 48.6%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07745439B2 |
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| 出典データセット | uspto-grants-2010_06 |
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| ORD ID | ord-df3eb7c1c5c742609cdcc4e6d4b8dcbe |
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| 出典メモ | uspto-grants-2010_06 |
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