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

HRID 476325

반응식

HRID 476325 반응식
[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]

참가 물질

6

반응물 4

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

생성물 1

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

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매2회

실험 절차

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%).

후처리

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

출처 및 근거

ORD 기록
ord-4b3913e785514510b517fe3b1864b195
출처 데이터셋
uspto-grants-2014_01
특허 번호
US08637710B2

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