Bromotrimethylsilane → HCID 14626581、化合物
反応式
[CH3:1][Si:2](Br)([CH3:4])[CH3:3].[F:6][C:7]1[CH:13]=[CH:12][CH:11]=[C:10]([F:14])[C:8]=1[NH2:9]>C1C=CC=CC=1>[CH3:1][Si:2]([CH3:4])([CH3:3])[NH:9][C:8]1[C:7]([F:6])=[CH:13][CH:12]=[CH:11][C:10]=1[F:14]参加物
4
実験手順
Trimethylsilyl bromide, 10.24 ml (77.5 mmole), was added to 6 ml (55.7 mmole) of 2,6-difluoroaniline in 70 ml of benzene. There was a slight exotherm and immediate precipitation. Triethylamine, 10.8 ml (77.5 mmole), was added and the mixture stirred at room temperature for 16 hours. The mixture was filtered and the solvent removed from the filtrate in vacuo. The product was purified as described in Example 1 to provide 8.85 g (51.1 mmole, 91.7 percent yield) of 99.3 percent pure N-trimethylsilyl-2,6-difluoroaniline as a colorless liquid, b.p. 89°-91° C. at 18 mm.
後処理
- customa slight exotherm and immediate precipitation
- additionTriethylamine, 10.8 ml (77.5 mmole), was added
- filtrationThe mixture was filtered
- customthe solvent removed from the filtrate in vacuo
- customThe product was purified
出典と根拠
- ORDレコード
- ord-acc4c52ac08c42c0bbe7795d2be0e690
- 出典データセット
- uspto-grants-1990_03
- 特許番号
- US04910306
反応ノート
読み込み中…