Benzene, 1-bromo-3,5-dimethyl- → 1,2-Bis(bis(3,5-dimethylphenyl)phosphino)benzene

HRID 476323

反応式

HRID 476323 の反応式
[CH3:1][C:2]1[CH:3]=[C:4](Br)[CH:5]=[C:6]([CH3:8])[CH:7]=1.[Mg].[CH3:11][C:12]1[CH:13]=[C:14]([Mg]Br)[CH:15]=[C:16]([CH3:18])[CH:17]=1.Cl[P:22](Cl)[C:23]1[CH:28]=[CH:27][CH:26]=[CH:25][C:24]=1[P:29](Cl)Cl>C1COCC1>[CH3:1][C:2]1[CH:3]=[C:4]([P:22]([C:4]2[CH:5]=[C:6]([CH3:8])[CH:7]=[C:2]([CH3:1])[CH:3]=2)[C:23]2[CH:28]=[CH:27][CH:26]=[CH:25][C:24]=2[P:29]([C:4]2[CH:5]=[C:6]([CH3:8])[CH:7]=[C:2]([CH3:1])[CH:3]=2)[C:14]2[CH:13]=[C:12]([CH3:11])[CH:17]=[C:16]([CH3:18])[CH:15]=2)[CH:5]=[C:6]([CH3:8])[CH:7]=1

参加物

6

反応物 4

HCID 136357Benzene, 1-bromo-3,5-dimethyl-HCID 33165621,2-Bis(dichlorophosphino)benzeneHCID 5462224MagnesiumHCID 178425074HCID 178425074、化合物

生成物 1

HCID 183243201,2-Bis(bis(3,5-dimethylphenyl)phosphino)benzene

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒2 回

実験手順

3,5-Dimethylbromobenzene (5.54 g, 29.93 mmol) was added dropwise to magnesium (1.07 g, 44.03 mmol) and THF (30 mL) in an argon atmosphere. The reaction mixture was cooled to ambient temperature and filtered, and the thus-obtained THF solution of 3,5-dimethylphenylmagnesium bromide, and 1,2-bis(dichlorophosphino)benzene (0.95 g, 3.39 mmol) were reacted as in Production Example 1. The reaction was allowed to proceed overnight at 60° C. After purification, the title compound was obtained as a white powder (1.45 g, yield 76%).

後処理

  1. filtrationfiltered
  2. customAfter purification

出典と根拠

ORDレコード
ord-54025fffc9d94247b3250ce08c963bc2
出典データセット
uspto-grants-2014_01
特許番号
US08637710B2

関連ノート

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