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1H-Indene, 2,3-dihydro-1,1,3,3,5-pentamethyl- → HCID 18177854、化合物

HRID 394920
ノート
印刷プレビュー

反応式

HRID 394920 の反応式
[CH3:1][C:2]1([CH3:14])[C:10]2[C:5](=[CH:6][C:7]([CH3:11])=[CH:8][CH:9]=2)[C:4]([CH3:13])([CH3:12])[CH2:3]1.[Br:15]N1C(=O)CCC1=O>C(Cl)(Cl)(Cl)Cl.N(C(C)(C)C#N)=NC(C)(C)C#N>[Br:15][CH2:11][C:7]1[CH:6]=[C:5]2[C:10](=[CH:9][CH:8]=1)[C:2]([CH3:14])([CH3:1])[CH2:3][C:4]2([CH3:13])[CH3:12]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

5

反応物 2

HCID 664691H-Indene, 2,3-dihydro-1,1,3,3,5-pentamethyl-HCID 67184N-bromobutanimide

生成物 1

HCID 18177854HCID 18177854、化合物収率 97.3%

試薬・触媒・溶媒 2

HCID 6547Azobisisobutyronitrile触媒HCID 5943Carbon Tetrachloride溶媒

反応条件

温度
0 °C

実験手順

10.0 g of 1,1,3,3,5-pentamethylindane were dissolved in 125 ml of carbontetrachloride and were added to the resulting solution, 9.92 g of N-bromosuccinimide and 35 mg of 2,2′-azobisisobutyronitrile (AIBN). The reaction mixture was heated to reflux for 5 hours. The reaction was cooled to 0° C. and the succinimide was filtered off. The resulting solution was concentrated in vacuo and the residue (14.7 g) was further dissolved in 150 ml of hexane. The precipitate was again removed by filtration and the solution was concentrated in vacuo, giving 13.8 g of 5-bromomethyl-1,1,3,3-tetramethylindane as a yellow oil.

後処理

  1. temperatureThe reaction mixture was heated
  2. temperatureto reflux for 5 hours
  3. filtrationthe succinimide was filtered off
  4. concentrationThe resulting solution was concentrated in vacuo
  5. dissolutionthe residue (14.7 g) was further dissolved in 150 ml of hexane
  6. customThe precipitate was again removed by filtration
  7. concentrationthe solution was concentrated in vacuo

出典と根拠

ORDレコード
ord-067ca15bb01347518ae9026f4b27f31b
出典データセット
uspto-grants-2003_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06603012B2

反応ノート

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