Carbon tetrabromide → 5-(1-Bromopropyl)-3-methylisoxazole
反応式
[CH3:1][C:2]1[CH:6]=[C:5]([CH:7](O)[CH2:8][CH3:9])[O:4][N:3]=1.C(Br)(Br)(Br)[Br:12].C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1>C1COCC1>[Br:12][CH:7]([C:5]1[O:4][N:3]=[C:2]([CH3:1])[CH:6]=1)[CH2:8][CH3:9]参加物
5
実験手順
To a solution of 1-(3-methylisoxazol-5-yl)propan-1-ol (0.589 g, 4.17 mmol) in 15 mL of THF was added CBr4 (1.730 g, 5.22 mmol) and triphenylphosphine (1.423 g, 5.42 mmol). The reaction mixture was stirred at room temperature for 3 h. The solid was filtered off, and washed with THF. The filtrate was concentrated and residue was purified by chromatography on silica gel, eluting with 5 to 30% EtOAc/hexane to provide the title compound. Mass Spectrum (ESI) m/z=204.2 (M+1).
後処理
- filtrationThe solid was filtered off
- washwashed with THF
- concentrationThe filtrate was concentrated
- customresidue was purified by chromatography on silica gel
- washeluting with 5 to 30% EtOAc/hexane
出典と根拠
- ORDレコード
- ord-86c4d6f88874492c8aeb34b80e129ee1
- 出典データセット
- uspto-grants-2016_03
- 特許番号
- US09296736B2
反応ノート
読み込み中…