2-Methyl-2-butene → HCID 22380897、化合物

HRID 895714

反応式

HRID 895714 の反応式
[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]

参加物

7

反応物 5

HCID 105532-Methyl-2-buteneHCID 516902Sodium ChlorateHCID 21885828Hydrate;hydrochlorideHCID 22380967HCID 22380967、化合物HCID 23673460Sodium Phosphate, Monobasic, Dihydrate

生成物 1

HCID 22380897HCID 22380897、化合物

試薬・触媒・溶媒 1

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

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-cd966038481b468884d58abc9f497da2
出典データセット
uspto-grants-2005_07
特許番号
US06916837B2

関連ノート

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