Phosphorus tribromide → HCID 11074939、化合物
反応式
[C:1]1([C:7]#[C:8]/[CH:9]=[CH:10]/[CH2:11]O)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.P(Br)(Br)[Br:14]>C1(C)C=CC=CC=1.C(OCC)(=O)C>[Br:14][CH2:11]/[CH:10]=[CH:9]/[C:8]#[C:7][C:1]1[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1参加物
5
実験手順
A solution of (E)-5-phenyl-pent-2-en-4-yn-1-ol (Method 1b) (980 mg, 6.2 mmol) in dry toluene (20 mL) was cooled on ice and phosphorus tribromide (0.59 mL, 6.2 mmol) added slowly. After 16 h at 5° C. the mixture was diluted with ethyl acetate and washed with water (×3). The organic phase was concentrated in vacuo and the residue extracted with heptane (×3). The combined heptane phases were concentrated in vacuo to give 900 mg of crude (E)-(5-bromo-pent-3-en-1-ynyl)-benzene. (According to NMR the product contained ˜5% of the (Z)-isomer).
後処理
- additionadded slowly
- washwashed with water (×3)
- concentrationThe organic phase was concentrated in vacuo
- extractionthe residue extracted with heptane (×3)
- concentrationThe combined heptane phases were concentrated in vacuo
出典と根拠
- ORDレコード
- ord-e9c520a55db84f41ada36f68a27a7a07
- 出典データセット
- uspto-grants-2003_05
- 特許番号
- US06569901B2
反応ノート
読み込み中…