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

HRID 476324

반응식

HRID 476324 반응식
[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]

참가 물질

6

반응물 4

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

생성물 1

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

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매2회

실험 절차

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%).

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-1e1949f1d47f4a6da13f1bcaf480c786
출처 데이터셋
uspto-grants-2014_01
특허 번호
US08637710B2

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