関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Aluminium lithium hydride | HCID 21226445 | — |
| 反応物 | methyl N-triphenylmethyl-5-benzimidazolecarboxylate | HCID 22710354 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | 1-Trityl-1H-benzimidazol-5-yl-methanol | HCID 23021539 | 86.4% |
反応手順
To an ice-cooled stirred suspension of the product of step b (3.61 g, 7.94 mmol) in THF (30 ml) was added dropwise a solution of lithium aluminium hydride (1.0M in THF, 10 ml, 10.0 mmol). The suspension was stirred at this temperature for 1 h and then was quenched with saturated aqueous ammonium chloride (100 ml). The aqueous solution was extracted thrice with ethyl acetate (100 ml) and the combined organic phases were washed with brine (200 ml). The organic phase was dried over magnesium sulfate and the filtrate was evaporated at reduced pressure and the residue recrystallised from ethyl acetate/hexane to afford the title compound (2.68 g, 79%). 1H NMR 7.89 (1H, s), 7.74 (1H, d, 8.4), 7.33-7.17 (17H, m), 6.44 (1H, d, 0.9), 4.45 (2H, d, 6), 1.37 (1H, t, 6).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US06878736B1 |
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| 出典データセット | uspto-grants-2005_04 |
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| ORD ID | ord-f7028a4a76bc44408a4da8a12b785a80 |
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| 出典メモ | uspto-grants-2005_04 |
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