Carbon tetrabromide → tert-Butyl 3-bromopropionate
反応式
[C:1]([O:5][C:6](=[O:10])[CH2:7][CH2:8]O)([CH3:4])([CH3:3])[CH3:2].C(Br)(Br)(Br)[Br:12].C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1>C(#N)C>[C:1]([O:5][C:6](=[O:10])[CH2:7][CH2:8][Br:12])([CH3:4])([CH3:3])[CH3:2]参加物
5
実験手順
3-Hydroxy-propionic acid tert-butyl ester is dissolved in acetonitrile and carbon tetrabromide and triphenylphosphine is added. The mixture is stirred at room temperature overnight. After this time the mixture is concentrated in vacuo. The gummy solid is triturated with hexanes and the liquid decanted, passed through pad of silica to remove any triphenylphosphine oxide, and concentrated in vacuo. 1H NMR (400 MHz, CHLOROFORM-d) ppm 1.3 (9H, s), 2.06-2.27 (2H, m), 4.07-4.25 (2H, m).
後処理
- concentrationAfter this time the mixture is concentrated in vacuo
- customThe gummy solid is triturated with hexanes
- customthe liquid decanted
- customto remove any triphenylphosphine oxide
- concentrationconcentrated in vacuo
出典と根拠
- ORDレコード
- ord-dcb257f0551e46a2852671ecd9f8e2c7
- 出典データセット
- uspto-grants-2014_01
- 特許番号
- US08629157B2
反応ノート
読み込み中…