1,2-Bis(dichlorophosphino)benzene → 1,2-Bis(bis(3,5-bis(2,6-dimethylphenyl)phenyl)phosphino)benzene

HRID 476326

反応式

HRID 476326 の反応式
Br[C:2]1[CH:7]=[C:6]([C:8]2[C:13]([CH3:14])=[CH:12][CH:11]=[CH:10][C:9]=2[CH3:15])[CH:5]=[C:4]([C:16]2[C:21]([CH3:22])=[CH:20][CH:19]=[CH:18][C:17]=2[CH3:23])[CH:3]=1.[Mg].Cl[P:26](Cl)[C:27]1[CH:32]=[CH:31][CH:30]=[CH:29][C:28]=1[P:33](Cl)Cl>C1COCC1>[CH3:15][C:9]1[CH:10]=[CH:11][CH:12]=[C:13]([CH3:14])[C:8]=1[C:6]1[CH:7]=[C:2]([P:26]([C:2]2[CH:3]=[C:4]([C:16]3[C:17]([CH3:23])=[CH:18][CH:19]=[CH:20][C:21]=3[CH3:22])[CH:5]=[C:6]([C:8]3[C:9]([CH3:15])=[CH:10][CH:11]=[CH:12][C:13]=3[CH3:14])[CH:7]=2)[C:27]2[CH:32]=[CH:31][CH:30]=[CH:29][C:28]=2[P:33]([C:2]2[CH:3]=[C:4]([C:16]3[C:17]([CH3:23])=[CH:18][CH:19]=[CH:20][C:21]=3[CH3:22])[CH:5]=[C:6]([C:8]3[C:9]([CH3:15])=[CH:10][CH:11]=[CH:12][C:13]=3[CH3:14])[CH:7]=2)[C:2]2[CH:3]=[C:4]([C:16]3[C:17]([CH3:23])=[CH:18][CH:19]=[CH:20][C:21]=3[CH3:22])[CH:5]=[C:6]([C:8]3[C:9]([CH3:15])=[CH:10][CH:11]=[CH:12][C:13]=3[CH3:14])[CH:7]=2)[CH:3]=[C:4]([C:16]2[C:21]([CH3:22])=[CH:20][CH:19]=[CH:18][C:17]=2[CH3:23])[CH:5]=1

参加物

5

反応物 3

HCID 33165621,2-Bis(dichlorophosphino)benzeneHCID 5462224MagnesiumHCID 154713392~5~-Bromo-1~2~,1~6~,3~2~,3~6~-tetramethyl-1~1~,2~1~:2~3~,3~1~-terphenyl

生成物 1

HCID 866548131,2-Bis(bis(3,5-bis(2,6-dimethylphenyl)phenyl)phosphino)benzene

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒2 回

実験手順

1-Bromo-3,5-bis(2,6-dimethylphenyl)benzene (2.74 g, 7.50 mmol) was added dropwise to magnesium (0.28 g, 11.52 mmol) and THF (10 mL) in an argon atmosphere. After the dropwise addition, the mixture was heated under reflux for 1 hour. The reaction mixture was cooled to ambient temperature and filtered, and the thus-obtained THF solution of 1-(3,5-bis(2,6-dimethylphenyl))magnesium bromide, and 1,2-bis(dichlorophosphino)benzene (0.28 g, 1.00 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 yellow powder (0.70 g, yield 62%).

後処理

  1. additionAfter the dropwise addition
  2. temperaturethe mixture was heated
  3. temperatureunder reflux for 1 hour
  4. filtrationfiltered
  5. customAfter purification

出典と根拠

ORDレコード
ord-0001196f94c947389f8fd96cac58b106
出典データセット
uspto-grants-2014_01
特許番号
US08637710B2

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