関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Sodium Bicarbonate | HCID 516892 | — |
| 反応物 | Borane;tetrahydrofuran | HCID 2723981 | — |
| 反応物 | (2R)-6-Iodochromane-2-carboxylic acid | HCID 9966213 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | [(2R)-6-iodo-3,4-dihydro-2H-chromen-2-yl]methanol | HCID 9943850 | — |
反応手順
A solution of borane-THF complex (1M in THF, 23.4 mmol, 1.2 eq) was added dropwise to a solution of (2R)-6-iodo-3,4-dihydro-2H-chromene-2-carboxylic acid (Example 7, 19.5 mmol, 1.0 eq.) in THF (45 mL) at 10° C. The resulting reaction mixture was stirred at 45° C. for 1.5 hours and was then cooled to 10° C. Next, water was added followed by saturated NaHCO3 solution. The resulting two-phase mixture was separated and aqueous phase was extracted with ethyl acetate. The combined organic extracts were washed with brine, dried over anhydrous sodium sulfate, concentrated to afford the product as a white solid in quantitative yield that was used without further purification.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US06699860B2 |
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| 出典データセット | uspto-grants-2004_03 |
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| ORD ID | ord-4f4291c27ea243a8876f5559000c68b7 |
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| 出典メモ | uspto-grants-2004_03 |
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