2-Bromo-2-methylpropionyl bromide → HCID 71089295, 화합물

HRID 1410322노트

반응식

HRID 1410322 반응식
[CH2:1]([C:15]1([CH2:28][CH2:29][CH2:30][CH2:31][CH2:32][CH2:33][CH2:34][CH2:35][CH2:36][CH2:37][CH2:38][CH2:39][CH2:40][CH3:41])[C:27]2[CH:26]=[CH:25][CH:24]=[CH:23][C:22]=2[C:21]2[C:16]1=[CH:17][CH:18]=[CH:19][CH:20]=2)[CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][CH2:12][CH2:13][CH3:14].Br[C:43]([CH3:48])([CH3:47])[C:44](Br)=[O:45].[Cl-].[Cl-].[Cl-].[Al+3]>C(=S)=S>[CH3:47][CH:43]1[C:44](=[O:45])[C:25]2=[CH:26][C:27]3[C:15]([CH2:1][CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][CH2:12][CH2:13][CH3:14])([CH2:28][CH2:29][CH2:30][CH2:31][CH2:32][CH2:33][CH2:34][CH2:35][CH2:36][CH2:37][CH2:38][CH2:39][CH2:40][CH3:41])[C:16]4[C:21]([C:22]=3[CH:23]=[C:24]2[CH2:48]1)=[CH:20][CH:19]=[CH:18][CH:17]=4

참가 물질

5

반응물 3

HCID 886852-Bromo-2-methylpropionyl bromideHCID 6451240Aluminum(III) ChlorideHCID 22568527HCID 22568527, 화합물

생성물 1

HCID 71089295HCID 71089295, 화합물수율 89.1%

시약·촉매·용매 1

HCID 6348Carbon Disulfide용매

실험 절차

A 5000 mL round flask was charged with 9,9-ditetradecyl-9H-fluorene (30 g, 53.7 mmol) and 2-bromo-2-methylpropanoyl bromide (12.7 g, 55.3 mmol), and then dissolved with 300 mL of carbon disulfide inputted thereto. Then, the reactor was cooled with ice water. Under nitrogen atmosphere, aluminum trichloride (15.7 g, 118.1 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 100 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, to thereby obtain 30.0 g of 2-methyl-9,9-ditetradecyl-2,3-dihydrocyclopenta[b]fluoren-1(9H)-one (yield: 89.1%) as highly viscous oil.

후처리

  1. customthe reaction was terminated by addition of 100 mL of distilled water
  2. washby washing with 500 mL of distilled water three times
  3. dry with materialThe organic layer was dried over magnesium sulfate
  4. customfollowed by removal of volatile materials
  5. customdrying

출처 및 근거

ORD 기록
ord-04ded70bd1aa4ce8a7facb0ca85e7f77
출처 데이터셋
uspto-grants-2014_12
특허 번호
US08921499B2

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