2-甲基-2-丁烯 → 5'-Nitro-2'-(6-cyano-2-naphthyloxy)-1,1'-biphenyl-2-carboxylic acid

HRID 895714

反应方程式

HRID 895714 反应方程式
[C:1]([C:3]1[CH:4]=[C:5]2[C:10](=[CH:11][CH:12]=1)[CH:9]=[C:8]([O:13][C:14]1[CH:19]=[CH:18][C:17]([N+:20]([O-:22])=[O:21])=[CH:16][C:15]=1[C:23]1[CH:28]=[CH:27][CH:26]=[CH:25][C:24]=1[CH:29]=[O:30])[CH:7]=[CH:6]2)#[N:2].CC(=CC)C.O.O.P([O-])(O)(O)=[O:39].[Na+].Cl([O-])(=O)=O.[Na+].O.Cl>C(#N)C.O>[N+:20]([C:17]1[CH:18]=[CH:19][C:14]([O:13][C:8]2[CH:7]=[CH:6][C:5]3[C:10](=[CH:11][CH:12]=[C:3]([C:1]#[N:2])[CH:4]=3)[CH:9]=2)=[C:15]([C:23]2[C:24]([C:29]([OH:39])=[O:30])=[CH:25][CH:26]=[CH:27][CH:28]=2)[CH:16]=1)([O-:22])=[O:21]

参与物

7

反应物 5

HCID 105532-甲基-2-丁烯HCID 516902氯酸钠HCID 21885828Hydrate;hydrochlorideHCID 223809674-(6-Cyano-2-naphthyloxy)-3-(2-formylphenyl)nitrobenzeneHCID 23673460二水合磷酸二氢钠

产物 1

HCID 223808975'-Nitro-2'-(6-cyano-2-naphthyloxy)-1,1'-biphenyl-2-carboxylic acid

试剂、催化剂与溶剂 1

HCID 18373917Acetonitrile--water (1/1)溶剂

实验过程

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.

后处理

  1. customAfter reaction for one hour at room temperature
  2. extractionextraction
  3. washThe ethyl acetate layer was washed with 1N hydrochloric acid water and saturated saline
  4. dry with materialdried over magnesium sulfate
  5. distillationthe solvent was distilled off

来源与证据

ORD记录
ord-cd966038481b468884d58abc9f497da2
来源数据集
uspto-grants-2005_07
专利号
US06916837B2

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