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四氧化硫 → (3-(Phenylamino)phenyl)methanol
参与物
| 角色 | 名称 | HCID | 投料 |
|---|---|---|---|
| 反应物 | 四氧化硫 | HCID 1118 | — |
| 反应物 | Methyl 3-(phenylamino)benzoate | HCID 614856 | — |
| 反应物 | 硼氢化钠 | HCID 4311764 | — |
| 溶剂 | (5BETA,17BETA)-17-羟基-17-(甲基-D3)-2'H-雄甾-2-烯并[3,2-C]吡唑-5'(1'H)-酮 | HCID 887 | — |
| 产物 | (3-(Phenylamino)phenyl)methanol | HCID 12882229 | 88.7% |
反应步骤
Under cooling with ice water, 7.2 g of sodium borohydride was gradually dropped into 4.5 g of methyl 3-anilinobenzoate dissolved in 20 ml of methanol. Then, the temperature was gradually raised and the reflux was carried out for 8 hours. The reaction mixture was poured into 10% H2SO4 aqueous solution which was being cooled with ice. 5.0 g of oily substance was obtained after the extraction with ether. In order to remove the remaining unreacted methyl ester, the hydrolysis was carried out with the addition of 5% KOH. The by-produced 3-anilinobenzoic acid was removed through alkali-washing to yield 3.5 g of 3-anilinobenzylalcohol.
来源与证据
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 专利号 | US04457940 |
| 来源数据集 | uspto-grants-1984_07 |
| ORD ID | ord-2f9d6bb0fe3c4d1e9c5e74fe1037625e |
| 来源说明 | uspto-grants-1984_07 |