Hydrochloric Acid → HCID 18761057、化合物

HRID 431413

反応式

HRID 431413 の反応式
Br[C:2]1[C:11]2[C:6](=[CH:7][CH:8]=[CH:9][CH:10]=2)[C:5]([C:12]2[C:21]3[C:16](=[CH:17][CH:18]=[CH:19][CH:20]=3)[CH:15]=[CH:14][CH:13]=2)=[CH:4][CH:3]=1.[Mg].[CH:23]1[C:36]2[C:35](=O)[C:34]3[C:29](=[CH:30][CH:31]=[CH:32][CH:33]=3)[CH2:28][C:27]=2[CH:26]=[CH:25][CH:24]=1.Cl>C(OCC)C.O1CCCC1>[CH:23]1[C:36]2[C:27](=[CH:28][C:29]3[C:34]([C:35]=2[C:15]2[C:16]4[C:21](=[CH:20][CH:19]=[CH:18][CH:17]=4)[C:12]([C:5]4[C:6]5[C:11](=[CH:10][CH:9]=[CH:8][CH:7]=5)[CH:2]=[CH:3][CH:4]=4)=[CH:13][CH:14]=2)=[CH:33][CH:32]=[CH:31][CH:30]=3)[CH:26]=[CH:25][CH:24]=1

参加物

7

反応物 4

HCID 313Hydrochloric AcidHCID 7018AnthroneHCID 5462224MagnesiumHCID 64258374-Bromo-1,1'-binaphthalene

生成物 1

HCID 18761057HCID 18761057、化合物

試薬・触媒・溶媒 2

HCID 3283Diethyl Ether溶媒HCID 8028Tetrahydrofuran溶媒

実験手順

4-bromo-1,1′-binaphthyl and magnesium were refluxed in diethylether for one hour, which was then added to a solution of anthrone in tetrahydrofuran. The resulting mixture was heated for two hours, which was then poured into diluted hydrochloric acid. After being extracted by diethylether, organic layer was separated and dried over magnesium sulfate. It was purified according to conventional method, whereby 1-(9-anthryl)-4-(1-naphthyl)-naphthalene was obtained. This was dissolved in chloroform to which was added two equivalent amounts of N-bromosuccinimide, and they were stirred at room temperature for one day. The product was purified according to conventional method and 1-(10-bromo-9-anthryl)-4-(4-bromo-1-naphthyl)-naphthalene was obtained. With this pdoruct, diphenylamine was reacted in nitrobenzene at 180° C. for 40 hours together with potasium carbonate and copper powder. After nitrobenzene was removed by vacuum distillation, the reaction mixture was purified according to conventional method, whereby the target compound (18) was obtained.

後処理

  1. temperatureThe resulting mixture was heated for two hours
  2. extractionAfter being extracted by diethylether, organic layer
  3. customwas separated
  4. dry with materialdried over magnesium sulfate
  5. customIt was purified

出典と根拠

ORDレコード
ord-1701c653018c44508d919f3fef87ec1e
出典データセット
uspto-grants-2003_12
特許番号
US06660408B1

関連ノート

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