反応式
[C:1]1([C:11]2[CH:16]=[CH:15][CH:14]=[CH:13][C:12]=2[CH3:17])[C:10]2[C:5](=[CH:6][CH:7]=[CH:8][CH:9]=2)[CH:4]=[CH:3][CH:2]=1.[Br:18]N1C(=O)CCC1=O>ClC(Cl)(Cl)Cl.N(C(C)(C)C#N)=NC(C)(C)C#N>[C:1]1([C:11]2[CH:16]=[CH:15][CH:14]=[CH:13][C:12]=2[CH2:17][Br:18])[C:10]2[C:5](=[CH:6][CH:7]=[CH:8][CH:9]=2)[CH:4]=[CH:3][CH:2]=1参加物
5
実験手順
114 g (0.52 mol) of 18 and 103 g (0.58 mol) of N-bromo-succinimide were dissolved in 2000 cm3 of tetrachloro-methane at room temperature, 3 g of azobisisobutyronitrile were added, and the mixture was refluxed for 4 hours. The succinimide which precipitated was filtered off, the solvent was removed in vacuo, and the residue was purified by filtration through 1000 g of silica gel (hexane/methylene chloride 9:1), giving 141 g (82%) of 19 as a colorless lachrymatory oil.
後処理
- temperaturethe mixture was refluxed for 4 hours
- customThe succinimide which precipitated
- filtrationwas filtered off
- customthe solvent was removed in vacuo
- filtrationthe residue was purified by filtration through 1000 g of silica gel (hexane/methylene chloride 9:1)
出典と根拠
- ORDレコード
- ord-11e0ec7f017a45db8fc648a77f1da37c
- 出典データセット
- uspto-grants-1998_11
- 特許番号
- US05840644
関連ノート
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