Sodium Hydroxide → HCID 66879256、化合物
反応式
C([O:4][C:5]1[CH:10]=[C:9]([Br:11])[CH:8]=[C:7]([F:12])[C:6]=1[O:13][CH2:14][C@H:15]1[CH2:17][O:16]1)(=O)C.[OH-].[Na+]>O1CCOCC1>[Br:11][C:9]1[CH:8]=[C:7]([F:12])[C:6]2[O:13][CH2:14][C@H:15]([CH2:17][OH:16])[O:4][C:5]=2[CH:10]=1参加物
4
実験手順
1-(5-bromo-3-fluoro-2-[(2R)-oxiran-2-ylmethoxy]phenyl acetate (crude, max 67 mmol) was stirred in dioxane at 0° C. NaOH (15%) was added until the mixture reached pH 14. The mixture was stirred for 30 min at RT and then concentrated. Water was added and the mixture extracted with EtOAc. The combined organic phases were washed with brine, dried (Na2SO4) and evaporated to dryness to give the crude title compound. Yield: 10.3 g. MS m/z (rel. intensity, 70 eV) 262 (M+, bp), 264 (M+, bp), 206 (70), 81 (58), 69 (55), 57 (53).
後処理
- concentrationconcentrated
- additionWater was added
- extractionthe mixture extracted with EtOAc
- washThe combined organic phases were washed with brine
- dry with materialdried (Na2SO4)
- customevaporated to dryness
出典と根拠
- ORDレコード
- ord-32a2f494200a4a5bbc14c29820a1e1b8
- 出典データセット
- uspto-grants-2013_09
- 特許番号
- US08524766B2
反応ノート
読み込み中…