Bromine → 2,4-Pentanedione, 3-(phenylmethylene)-

HRID 1975714

反応式

HRID 1975714 の反応式
[CH2:1]([CH:8]([C:12](=[O:14])[CH3:13])[C:9](=[O:11])[CH3:10])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.BrBr>ClCCl>[CH:1](=[C:8]([C:9](=[O:11])[CH3:10])[C:12](=[O:14])[CH3:13])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1

参加物

4

反応物 2

HCID 24408BromineHCID 977572,4-Pentanedione, 3-benzyl-

生成物 1

HCID 957822,4-Pentanedione, 3-(phenylmethylene)-

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

反応条件

温度
0 °C

実験手順

To a solution containing 6.3 g of 3-benzyl-2,4-pentanedione in 50 ml of dichloromethane was gradually added 5.3 g of bromine in 20 ml of dichloromethane under cooling (0°-5° C.). The solution was stirred for 10 min. at 0° C. and the solvent evaporated in vacuo. The residue was dissolved in 100 ml of pyridine and refluxed for 30 min. Pyridine was evaporated in vacuo, the residue was dissolved in dichloromethane and washed first with 6M hydrochloric acid and then with 2.6M NaOH. The solvent was evaporated and the residue distilled in vacuo. Bp 186°-188° C./16 mm, yield 1.2 g.

後処理

  1. temperatureunder cooling (0°-5° C.)
  2. customthe solvent evaporated in vacuo
  3. dissolutionThe residue was dissolved in 100 ml of pyridine
  4. temperaturerefluxed for 30 min
  5. customPyridine was evaporated in vacuo
  6. dissolutionthe residue was dissolved in dichloromethane
  7. washwashed first with 6M hydrochloric acid
  8. customThe solvent was evaporated
  9. distillationthe residue distilled in vacuo

出典と根拠

ORDレコード
ord-9ef2542a0bc54e89bad3bec9512d3871
出典データセット
uspto-grants-1994_02
特許番号
US05288750

関連ノート

読み込み中…