Carbon tetrabromide → HCID 90203452、化合物
反応式
[Cl:1][C:2]1[CH:7]=[C:6]([CH2:8]O)[C:5]([Cl:10])=[CH:4][N:3]=1.[Br:11]C(Br)(Br)Br.C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1>C(Cl)Cl>[Br:11][CH2:8][C:6]1[C:5]([Cl:10])=[CH:4][N:3]=[C:2]([Cl:1])[CH:7]=1参加物
5
反応条件
- 温度
- 0 °C
実験手順
To a suspension of 2,5-dichloro-4-pyridinemethanol (CAN 866039-42-1, 1.10 g, 6.18 mmol) in DCM (25 mL) was added at 0° C. with stirring tetrabromomethane (2.05 g, 6.18 mmol) and a solution of triphenylphosphine (1.62 g, 6.18 mmol) in DCM (5 mL). The resulting mixture was stirred at 0° C. for 1 h and concentrated. The residue was purified by flash chromatography (silica, heptane/ethyl acetate gradient) to give the title compound (619 mg, 42%) as yellow oil. LC-MS (UV peak area, m/z) 98%, 241.0 (MH+).
後処理
- concentrationconcentrated
- customThe residue was purified by flash chromatography (silica, heptane/ethyl acetate gradient)
出典と根拠
- ORDレコード
- ord-991eca45e8a84ea696d0e132e31dab7e
- 出典データセット
- uspto-grants-2016_08
- 特許番号
- US09409866B2
反応ノート
読み込み中…