参与物
| 角色 | 名称 | HCID | 投料 |
|---|
| 反应物 | 氯化亚锡 | HCID 24479 | — |
| 反应物 | 3-氨基-4-甲基苯甲酸 | HCID 75568 | — |
| 反应物 | 亚硝酸钠 | HCID 23668193 | — |
| 溶剂 | 醋酸 | HCID 176 | — |
| 溶剂 | 海萝胶 | HCID 313 | — |
| 溶剂 | 聚[6-[4-(4-氰基苯基)苯氧基]己基甲基丙烯酸酯] | HCID 962 | — |
| 产物 | 3-肼基-4-甲基苯甲酸盐酸盐 | HCID 56777508 | — |
反应步骤
A solution of 2.74 g of NaNO2 in 28 ml of water is added over 30 minutes to a solution, cooled to -5° C., of 5 g of 3-amino-4-methylbenzoic acid in 120 ml of concentrated HCl and 40 ml AcOH, and the mixture is left stirring for 1 hour 20 minutes at 0° C. After cooling to -10° C., a solution of 27.6 g of SnCl2 ·2H2O in 28 ml of concentrated HCl is added slowly. After stirring for 1 hour at RT, filtration, washing of the precipitate with 5 ml of 1N HCl and drying over P2O5 under vacuum, 6.15 g of the expected product are obtained.
来源与证据
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 专利号 | US05723483 |
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| 来源数据集 | uspto-grants-1998_03 |
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| ORD ID | ord-e46e69b904a7491db50b6afa5f24b6f5 |
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| 来源说明 | uspto-grants-1998_03 |
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