2-Bromo-2-methylpropionyl bromide → HCID 71089296、化合物

HRID 2273374ノート

反応式

HRID 2273374 の反応式
[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]

参加物

5

反応物 3

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

生成物 1

HCID 71089296HCID 71089296、化合物収率 93.6%

試薬・触媒・溶媒 1

HCID 6348Carbon Disulfide溶媒

実験手順

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

後処理

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

出典と根拠

ORDレコード
ord-a952a942402040688c5afb49edfcb0ac
出典データセット
uspto-grants-2015_09
特許番号
US09120884B2

反応ノート

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