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HRID 747359作成日:2026年10月25日

Methanol → HCID 178419086、化合物

https://huagongshe.com/reaction/747359

反応式

関与物質

役割名称HCID仕込み量
反応物MethanolHCID 887—
反応物Borane;tetrahydrofuranHCID 2723981—
反応物HCID 178418543HCID 178418543—
溶媒TetrahydrofuranHCID 8028—
生成物HCID 178419086HCID 17841908629%

反応条件

温度80 °C

反応手順

To a suspension of 2-Hydroxynicotinic acid (1.01 g, 7.26 mmol) in THF (2 mL) was added BH3.THF (1.0 m in THF, 18 mL, 18 mmol) and the mixture was heated to 80° C. for 18 hours. MeOH (2 mL) was added and the mixture was heated to 80° C. for an additional 2 hours before being cooled to room temperature and concentrated under reduced pressure. The resultant crude syrup was repeatedly dissolved in MeOH (5 mL) and concentrated (3×). Purification by column chromatography on silica gel (20:1—CH2Cl2:MeOH) afforded the desired alcohol (260 mg, 29%) as a white solid. 1H NMR (CD3OD) δ 4.50 (s, 2H), 6.43 (t, 1H, J=6.6 Hz), 7.34 (d, 1H, J=4.5 Hz), 7.65 (d, 1H, J=6.3 Hz).

情報源と証拠

DOI10.6084/m9.figshare.5104873.v1
特許番号US07396840B2
出典データセットuspto-grants-2008_07
ORD IDord-89d938e29a12449fb5640ff2bf0912aa
出典メモuspto-grants-2008_07