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Acetone → 2-Hydroxymethyl-5-morpholin-4-yl-phenol
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Acetone | HCID 180 | — |
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Sodium borohydride | HCID 4311764 | — |
| 反応物 | 2-Hydroxy-4-morpholin-4-yl-benzaldehyde | HCID 9815659 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 2-Hydroxymethyl-5-morpholin-4-yl-phenol | HCID 9920743 | 37.2% |
反応手順
A solution of sodium borohydride (NaBH4) (0.66 g, 17 mmol) in water (25 mL) was treated with 4-morpholinylsalicylaldehyde (1.8 g, 9 mmol) in small portions over 30 min and stirred at room temperature for 3 h. The reaction was quenched with acetone (5.1 mL, 100 mmol), acidified to pH 7 with 7.8 mL of 5% hydrochloric acid (aqueous) and extracted with chloroform (CHCl3) (2×100 mL). The combined CHCl3 extracts were dried over sodium sulfate (Na2SO4) and concentrated in vacuo to yield 0.7 g of pale yellow solid which was purified by trituration with 60/40 CHCl3/ethyl acetate (EtOAc) to yield the product as a white solid (0.25 g).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07179912B2 |
| 出典データセット | uspto-grants-2007_02 |
| ORD ID | ord-fddba469efab4fe9be35ef6e6ffaaf17 |
| 出典メモ | uspto-grants-2007_02 |