Nitrogen → (2-(Methoxymethyl)oxazol-4-yl)methanol
反応式
N#N.[CH3:3][O:4][CH2:5][C:6]1[O:7][CH:8]=[C:9]([C:11](OC)=[O:12])[N:10]=1.[H-].[H-].[H-].[H-].[Li+].[Al+3].O>C1COCC1>[CH3:3][O:4][CH2:5][C:6]1[O:7][CH:8]=[C:9]([CH2:11][OH:12])[N:10]=1参加物
反応条件
- 温度
- 0 °C
実験手順
In a flame dried round-bottomed flask equipped with a magnetic stir bar and under inert atmosphere (N2), a solution of methyl 2-(methoxymethyl)oxazole-4-carboxylate (192 mg, 1.12 mmol) in THF (11 mL) was treated dropwise at 0° C. with LiAlH4 (1.35 mL of a 1.0 M solution in THF, 1.35 mmol) and the resulting solution was stirred for 20 min at 0° C. The reaction mixture was carefully treated with water (1.0 mL) 1N NaOH (1.0 mL) followed by water (1.0 mL) and the mixture was stirred for 1 h at rt. The resulting suspension was filtered, extracted with EA and the combined org. layers were dried over MgSO4, filtered and the solvent was removed under reduced pressure to give the title compound as a brown oil. LC-MS-conditions 07: tR=0.33 min; [M+H]+=144.08.
後処理
- stirringthe mixture was stirred for 1 h at rt
- filtrationThe resulting suspension was filtered
- extractionextracted with EA
- dry with materiallayers were dried over MgSO4
- filtrationfiltered
- customthe solvent was removed under reduced pressure
出典と根拠
- ORDレコード
- ord-d8bd6106f0cd494e8e10357b93122bd2
- 出典データセット
- uspto-grants-2014_09
- 特許番号
- US08846733B2
反応ノート
読み込み中…