1,2-Bis(dichlorophosphino)benzene → 1,2-Bis(bis(3,5-diisopropylphenyl)phosphino)benzene

HRID 476324

反応式

HRID 476324 の反応式
[CH:1]([C:4]1[CH:5]=[C:6](Br)[CH:7]=[C:8]([CH:10]([CH3:12])[CH3:11])[CH:9]=1)([CH3:3])[CH3:2].[Mg].[CH:15]([C:18]1[CH:19]=[C:20]([Mg]Br)[CH:21]=[C:22]([CH:24]([CH3:26])[CH3:25])[CH:23]=1)([CH3:17])[CH3:16].Cl[P:30](Cl)[C:31]1[CH:36]=[CH:35][CH:34]=[CH:33][C:32]=1[P:37](Cl)Cl>C1COCC1>[CH:1]([C:4]1[CH:5]=[C:6]([P:30]([C:6]2[CH:5]=[C:4]([CH:1]([CH3:2])[CH3:3])[CH:9]=[C:8]([CH:10]([CH3:12])[CH3:11])[CH:7]=2)[C:31]2[CH:36]=[CH:35][CH:34]=[CH:33][C:32]=2[P:37]([C:6]2[CH:7]=[C:8]([CH:10]([CH3:12])[CH3:11])[CH:9]=[C:4]([CH:1]([CH3:3])[CH3:2])[CH:5]=2)[C:20]2[CH:19]=[C:18]([CH:15]([CH3:17])[CH3:16])[CH:23]=[C:22]([CH:24]([CH3:26])[CH3:25])[CH:21]=2)[CH:7]=[C:8]([CH:10]([CH3:12])[CH3:11])[CH:9]=1)([CH3:3])[CH3:2]

参加物

6

反応物 4

HCID 33165621,2-Bis(dichlorophosphino)benzeneHCID 5462224MagnesiumHCID 116300913,5-DiisopropylbromobenzeneHCID 178439359HCID 178439359、化合物

生成物 1

HCID 866548121,2-Bis(bis(3,5-diisopropylphenyl)phosphino)benzene収率 74%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒2 回

実験手順

3,5-Diisopropylbromobenzene (3.04 g, 12.60 mmol) was added dropwise to magnesium (0.48 g, 19.75 mmol) and THF (7 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 3,5-diisopropylphenylmagnesium bromide, and 1,2-bis(dichlorophosphino)benzene (0.45 g, 1.61 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 oily substance (1.18 g, yield 74%).

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-1e1949f1d47f4a6da13f1bcaf480c786
出典データセット
uspto-grants-2014_01
特許番号
US08637710B2

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