1-Bromo-3,5-di-tert-butylbenzene → 1,2-Bis(bis(3,5-di-tert-butylphenyl)phosphaneyl)benzene

HRID 476325

反応式

HRID 476325 の反応式
[C:1]([C:5]1[CH:6]=[C:7](Br)[CH:8]=[C:9]([C:11]([CH3:14])([CH3:13])[CH3:12])[CH:10]=1)([CH3:4])([CH3:3])[CH3:2].[Mg].[C:17]([C:21]1[CH:22]=[C:23]([Mg]Br)[CH:24]=[C:25]([C:27]([CH3:30])([CH3:29])[CH3:28])[CH:26]=1)([CH3:20])([CH3:19])[CH3:18].Cl[P:34](Cl)[C:35]1[CH:40]=[CH:39][CH:38]=[CH:37][C:36]=1[P:41](Cl)Cl>C1COCC1>[C:1]([C:5]1[CH:6]=[C:7]([P:34]([C:7]2[CH:6]=[C:5]([C:1]([CH3:3])([CH3:2])[CH3:4])[CH:10]=[C:9]([C:11]([CH3:14])([CH3:13])[CH3:12])[CH:8]=2)[C:35]2[CH:40]=[CH:39][CH:38]=[CH:37][C:36]=2[P:41]([C:7]2[CH:8]=[C:9]([C:11]([CH3:14])([CH3:13])[CH3:12])[CH:10]=[C:5]([C:1]([CH3:4])([CH3:3])[CH3:2])[CH:6]=2)[C:23]2[CH:22]=[C:21]([C:17]([CH3:20])([CH3:19])[CH3:18])[CH:26]=[C:25]([C:27]([CH3:30])([CH3:29])[CH3:28])[CH:24]=2)[CH:8]=[C:9]([C:11]([CH3:14])([CH3:13])[CH3:12])[CH:10]=1)([CH3:4])([CH3:3])[CH3:2]

参加物

6

反応物 4

HCID 6201361-Bromo-3,5-di-tert-butylbenzeneHCID 33165621,2-Bis(dichlorophosphino)benzeneHCID 5462224MagnesiumHCID 178441125HCID 178441125、化合物

生成物 1

HCID 566468691,2-Bis(bis(3,5-di-tert-butylphenyl)phosphaneyl)benzene

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒2 回

実験手順

3,5-Di-tert-butylbromobenzene (12.50 g, 46.43 mmol) was added dropwise to magnesium (1.70 g, 69.96 mmol) and THF (50 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-di-tert-butylphenylmagnesium bromide, and 1,2-bis(dichlorophosphino)benzene (2.00 g, 7.15 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 (4.66 g, yield 73%).

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-4b3913e785514510b517fe3b1864b195
出典データセット
uspto-grants-2014_01
特許番号
US08637710B2

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