Phosphorus tribromide → HCID 19861650、化合物
反応式
P(Br)(Br)[Br:2].[Br:5][C:6]1[C:7]([CH2:16]O)=[CH:8][C:9]2[C:14]([CH:15]=1)=[CH:13][CH:12]=[CH:11][CH:10]=2>C(OCC)C>[Br:5][C:6]1[C:7]([CH2:16][Br:2])=[CH:8][C:9]2[C:14]([CH:15]=1)=[CH:13][CH:12]=[CH:11][CH:10]=2参加物
4
実験手順
PBr3 (3.7 mL, 0.039 mol) was added dropwise to a suspension of 3-bromo-2-naphthalenyl methanol (8.55 g, 0.036 mol) and diethyl ether (80 mL) at 0° C. After 1 hour, the reaction was concentrated and partitioned between CH2Cl2 and H2O. The organic layer was separated and dried over MgSO4. Concentration in vacuo afforded 3-bromo-2-bromomethylnaphthalene as a crude product (10.6 g). The crude product was flash chromatographed on silica gel to afford the pure product as an off-white powder (6.0 g, m.p. 110°-111° C., yield 56%).
後処理
- concentrationthe reaction was concentrated
- custompartitioned between CH2Cl2 and H2O
- customThe organic layer was separated
- dry with materialdried over MgSO4
- concentrationConcentration in vacuo
出典と根拠
- ORDレコード
- ord-95b623ee845b4e4bb3f70767464c035d
- 出典データセット
- uspto-grants-1990_03
- 特許番号
- US04910019
反応ノート
読み込み中…