Phosphorus tribromide → 1372891-51-4
反応式
[F:1][C:2]1[C:3]([CH2:9]O)=[N:4][CH:5]=[CH:6][C:7]=1[CH3:8].P(Br)(Br)[Br:12]>C1COCC1>[Br:12][CH2:9][C:3]1[C:2]([F:1])=[C:7]([CH3:8])[CH:6]=[CH:5][N:4]=1参加物
4
実験手順
Intermediate 6 ((3-fluoro-4-methyl-2-pyridinyl)methanol, 246 mg, 1.743 mmol) was dissolved in 10 mL of anhydrous THF. Phosphorous tribromide (ALDRICH, 519 mg, 1.917 mmol) was added. Reaction mixture was stirred at room temperature overnight. Solvent was evaporated and residue was partitioned between Et2O and NaHCO3 (aqueous saturated solution). Organic layer was dried over MgSO4 (anh), filtered and concentrated to give the title compound (372 mg, quantitative yield). 1H NMR (300 MHz, DMSO-d6) δ ppm: 8.23-8.24 (m, 1H), 7.34-7.37 (m, 1H), 4.66 (s, 2H), 2.28 (s, 3H). [ES+MS] m/z 204 (M).
後処理
- customReaction mixture
- customSolvent was evaporated
- customresidue was partitioned between Et2O and NaHCO3 (aqueous saturated solution)
- dry with materialOrganic layer was dried over MgSO4 (anh)
- filtrationfiltered
- concentrationconcentrated
出典と根拠
- ORDレコード
- ord-00520d7642d740b1abd77cf5b68907aa
- 出典データセット
- uspto-grants-2014_07
- 特許番号
- US08779153B2
反応ノート
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