HCID 59255222、化合物 → HCID 59255438、化合物
反応式
[O:1]([C:8]1[CH:9]=[C:10]([CH2:14][OH:15])[CH:11]=[N:12][CH:13]=1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1>[O-2].[O-2].[Mn+4].C(Cl)Cl>[O:1]([C:8]1[CH:9]=[C:10]([CH:14]=[O:15])[CH:11]=[N:12][CH:13]=1)[C:2]1[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=1参加物
4
実験手順
To a methylene chloride (20 mL) solution of (5-phenoxy-pyridin-3-yl)-methanol (756 mg, 3.76 mmol) described in Manufacturing Example 145-1-2 was added manganese(IV) dioxide (3.27 g, 37.6 mmol), which was stirred for 2 hours at room temperature. The insolubles were removed by filtrating through a Celite pad, after which the filtrate was concentrated under a reduced pressure. The residue was purified by silica gel column chromatography (heptane:ethyl acetate=2:1 to 1:1) to obtain the title compound (607 mg, 81%).
後処理
- customThe insolubles were removed
- filtrationby filtrating through a Celite pad
- concentrationafter which the filtrate was concentrated under a reduced pressure
- customThe residue was purified by silica gel column chromatography (heptane:ethyl acetate=2:1 to 1:1)
出典と根拠
- ORDレコード
- ord-9a83979e17024d3f9b0ea333190fd6bf
- 出典データセット
- uspto-grants-2012_04
- 特許番号
- US08153662B2
反応ノート
読み込み中…