1,3-Cyclohexanedione → 2-Bromocyclohexane-1,3-dione

HRID 2383417ノート

反応式

HRID 2383417 の反応式
[C:1]1(=[O:8])[CH2:6][CH2:5][CH2:4][C:3](=[O:7])[CH2:2]1.[Br:9]Br>ClCCl>[Br:9][CH:2]1[C:3](=[O:7])[CH2:4][CH2:5][CH2:6][C:1]1=[O:8]

参加物

4

反応物 2

HCID 104341,3-CyclohexanedioneHCID 24408Bromine

生成物 1

HCID 27704762-Bromocyclohexane-1,3-dione収率 82.3%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

実験手順

To a stirred solution of 1,3 Cyclohexandione (10 g, 89 mmol) in dichloromethane (22 mL) at 0° C. was added a solution of bromine (3.8 mL, 89 mmol) in dichloromethane (3 mL) over a period of 10 minutes. The reaction mixture was stirred at room temperature for 1.5 hours. The reaction mixture was filtered and the residue washed with hexane (200 mL). The residue was taken into water (75 mL) and heated at 80° C. for 30 minutes. It was cooled to room temperature, filtered and dried under reduced pressure to give the desired product (14 g, 82%) as a solid. ESMS [M+H]: 191.

後処理

  1. filtrationThe reaction mixture was filtered
  2. washthe residue washed with hexane (200 mL)
  3. temperatureheated at 80° C. for 30 minutes
  4. temperatureIt was cooled to room temperature
  5. filtrationfiltered
  6. customdried under reduced pressure

出典と根拠

ORDレコード
ord-77fd35eb05c743b7834e9c0122742e7f
出典データセット
uspto-grants-2012_09
特許番号
US08263610B2

反応ノート

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