2-Bromo-2-methylpropionyl bromide → HCID 71089296, 화합물

HRID 1055281노트

반응식

HRID 1055281 반응식
[CH2:1]([C:7]1([CH2:20][CH2:21][CH2:22][CH2:23][CH2:24][CH3:25])[C:19]2[CH:18]=[CH:17][CH:16]=[CH:15][C:14]=2[C:13]2[C:8]1=[CH:9][CH:10]=[CH:11][CH:12]=2)[CH2:2][CH2:3][CH2:4][CH2:5][CH3:6].Br[C:27]([CH3:32])([CH3:31])[C:28](Br)=[O:29].[Cl-].[Cl-].[Cl-].[Al+3]>C(=S)=S>[CH2:20]([C:7]1([CH2:1][CH2:2][CH2:3][CH2:4][CH2:5][CH3:6])[C:19]2[CH:18]=[C:17]3[C:28](=[O:29])[CH:27]([CH3:32])[CH2:31][C:16]3=[CH:15][C:14]=2[C:13]2[C:8]1=[CH:9][CH:10]=[CH:11][CH:12]=2)[CH2:21][CH2:22][CH2:23][CH2:24][CH3:25]

참가 물질

5

반응물 3

HCID 886852-Bromo-2-methylpropionyl bromideHCID 51284499,9-dihexylfluoreneHCID 6451240Aluminum(III) Chloride

생성물 1

HCID 71089296HCID 71089296, 화합물수율 93.6%

시약·촉매·용매 1

HCID 6348Carbon Disulfide용매

실험 절차

9,9-dihexyl-9H-fluorene (79 g, 236.2 mmol) and 2-bromo-2-methylpropanoyl bromide (54.3 g, 236.2 mmol) were injected into a 2000 mL round flask and then dissolved by adding 600 mL of carbon disulfide inputted thereto. Then, the reactor was cooled with ice water. Aluminum trichloride (78.7 g, 590.4 mmol) was slowly added thereto in ten lots over 2 hours under nitrogen atmosphere. Then, after the mixture was stirred at room temperature for 8 hours, the reaction was terminated by adding of 500 mL of distilled water, followed by washing with 500 mL of distilled water three times. The organic layer was dried over magnesium sulfate, followed by removal of volatile materials and drying, thereby obtaining 89.0 g of 9,9-dihexyl-2-methyl-2,3-dihydrocyclopenta[b]fluoren-1(9H)-one (yield: 93.6%) as highly viscous oil.

후처리

  1. dissolutiondissolved
  2. customthe reaction was terminated
  3. additionby adding of 500 mL of distilled water
  4. washby washing with 500 mL of distilled water three times
  5. dry with materialThe organic layer was dried over magnesium sulfate
  6. customfollowed by removal of volatile materials
  7. customdrying

출처 및 근거

ORD 기록
ord-7e63d456170148a4ab568bdc32750bd4
출처 데이터셋
uspto-grants-2016_07
특허 번호
US09394388B2

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