参与物
| 角色 | 名称 | HCID | 投料 |
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| 反应物 | 2-甲基-2-丁烯 | HCID 10553 | — |
| 反应物 | 氯酸钠 | HCID 516902 | — |
| 反应物 | Hydrate;hydrochloride | HCID 21885828 | — |
| 反应物 | 4-(6-Cyano-2-naphthyloxy)-3-(2-formylphenyl)nitrobenzene | HCID 22380967 | — |
| 反应物 | 二水合磷酸二氢钠 | HCID 23673460 | — |
| 溶剂 | Acetonitrile--water (1/1) | HCID 18373917 | — |
| 产物 | 5'-Nitro-2'-(6-cyano-2-naphthyloxy)-1,1'-biphenyl-2-carboxylic acid | HCID 22380897 | — |
反应步骤
The compound (4-(6-cyano-2-naphthyloxy)-3-(2-formylphenyl)nitrobenzene) (800 mg) obtained in a previous production example, 2-methyl-2-butene (1.4 ml) and sodium dihydrogen phosphate dihydrate (2 g) were dissolved in acetonitrile:water (2:1, 50 ml) and then sodium chlorate (1 g) was added. After reaction for one hour at room temperature, 1 N hydrochloric acid water was added and extraction was performed with ethyl acetate. The ethyl acetate layer was washed with 1N hydrochloric acid water and saturated saline and then dried over magnesium sulfate, and the solvent was distilled off to obtain 5′-nitro-2′-(6-cyano-2-naphthyloxy)-1,1′-biphenyl-2-carboxylic acid (800 mg). This was dissolved in toluene without purification and subjected to the same process as in Production Example 1 to obtain t-butyl 2′-(6-cyano-2-naphthyloxy)-5′-nitro-1,1′-biphenyl-2-carboxylate.
来源与证据
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 专利号 | US06916837B2 |
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| 来源数据集 | uspto-grants-2005_07 |
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| ORD ID | ord-cd966038481b468884d58abc9f497da2 |
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| 来源说明 | uspto-grants-2005_07 |
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