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Sodium borohydride → (4-[1,3]Dioxolan-2-yl-3-fluoro-phenyl)-methanol
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Sodium borohydride | HCID 4311764 | — |
| 反応物 | 4-[1,3]Dioxolan-2-yl-3-fluoro-benzaldehyde | HCID 59255459 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 生成物 | (4-[1,3]Dioxolan-2-yl-3-fluoro-phenyl)-methanol | HCID 59255152 | 24.2% |
反応手順
To a methanol solution (200 mL) of 4-[1,3]dioxolan-2-yl-3-fluoro-benzaldehyde (10 g, 50.9 mmol) described in Manufacturing Example 204-1-2 was added sodium borohydride (2.12 g, 56 mmol), which was stirred for 1 hour at room temperature. This mixture was partitioned into ethyl acetate and water. The organic layer was separated, washed with water, dried over anhydrous magnesium sulfate, and filtered. The filtrate was concentrated under a reduced pressure, and the residue was purified by NH silica gel column chromatography (ethyl acetate:heptane=1:1) to obtain the title compound (2.44 g, 24%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07691882B2 |
| 出典データセット | uspto-grants-2010_04 |
| ORD ID | ord-b0bd8521f8084482bca19d87608b7854 |
| 出典メモ | uspto-grants-2010_04 |