Water → HCID 136093607、化合物
反応式
[CH:1]12[CH2:10][CH:5]3[CH2:6][CH:7]([CH2:9][CH:3]([CH2:4]3)[C:2]1=[C:11]1[C:16]3[CH:17]=[CH:18][CH:19]=[CH:20][C:15]=3[O:14][C:13]([C:21]3[CH:26]=[CH:25][C:24]([O:27]C)=[CH:23][CH:22]=3)=[N:12]1)[CH2:8]2.B(I)(I)I.O>C(Cl)Cl>[CH:1]12[CH2:10][CH:5]3[CH2:6][CH:7]([CH2:9][CH:3]([CH2:4]3)[C:2]1=[C:11]1[C:16]3[CH:17]=[CH:18][CH:19]=[CH:20][C:15]=3[O:14][C:13]([C:21]3[CH:26]=[CH:25][C:24]([OH:27])=[CH:23][CH:22]=3)=[N:12]1)[CH2:8]2参加物
5
実験手順
A solution of 6 mmol 4-adamantylidene-2-(4'-methoxyphenyl)-4H-1,3-benzoxazine in 20 ml absolute methylene chloride is added dropwise to a solution of 12 mmol boron triiodide while stirring at -25° C. with the exclusion of air and water. The mixture is heated to room temperature within one hour and stirred for a further 4 hours. After admixing with 50 ml water the organic phase is separated and dried over sodium sulfate. The solvent is removed by distillation. The oily residue is separated by column chromatography (silica gel: ethyl acetate/petroleum ether 1:3).
後処理
- customis separated
- dry with materialdried over sodium sulfate
- customThe solvent is removed by distillation
- customThe oily residue is separated by column chromatography (silica gel: ethyl acetate/petroleum ether 1:3)
出典と根拠
- ORDレコード
- ord-5c659b3a32234956bf5e09651599bcd3
- 出典データセット
- uspto-grants-2000_08
- 特許番号
- US06107036
反応ノート
読み込み中…