Carbon tetrabromide → 5-Bromo-2-(bromomethyl)-1,3-difluorobenzene
反応式
[Br:1][C:2]1[CH:9]=[C:8]([F:10])[C:5]([CH2:6]O)=[C:4]([F:11])[CH:3]=1.C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.C(Br)(Br)(Br)[Br:32]>C1COCC1>[Br:1][C:2]1[CH:9]=[C:8]([F:10])[C:5]([CH2:6][Br:32])=[C:4]([F:11])[CH:3]=1参加物
5
実験手順
To a cooled (0° C.) solution of 4 g (17.6 mmol) 4-bromo-2,6-difluorobenzyl alcohol in 50 ml THF, 7 g (26.4 mmol) triphenylphosphine and 8.83 g (26.4 mmol) carbon tetrabromide are added with stirring. Stirring is continued for 10 min at 0° C. and for 1 h at room temperature. After that the reaction mixture is filtered and the filtrate is concentrated in vacuo. The residue is purified by chromatography (silicagel, hexane) to afford the title compound as yellowish oil.
後処理
- additionare added
- stirringStirring
- filtrationAfter that the reaction mixture is filtered
- concentrationthe filtrate is concentrated in vacuo
- customThe residue is purified by chromatography (silicagel, hexane)
出典と根拠
- ORDレコード
- ord-0d02b1b38e944b19896040d89c32db47
- 出典データセット
- uspto-grants-2014_01
- 特許番号
- US08629168B2
反応ノート
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