Nitrogen → 2-(Chloromethyl)-4-(ethoxymethyl)oxazole
反応式
N#N.[Cl:3][CH2:4][C:5]1[O:6][CH:7]=[C:8]([CH2:10][OH:11])[N:9]=1.[CH2:12](I)[CH3:13]>C(Cl)Cl>[Cl:3][CH2:4][C:5]1[O:6][CH:7]=[C:8]([CH2:10][O:11][CH2:12][CH3:13])[N:9]=1参加物
5
反応条件
- 温度
- 40 °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 (2-(chloromethyl)oxazol-4-yl)methanol (500 mg, 3.39 mmol) in CH2Cl2 (2.0 mL) was treated with EtI (0.28 mL, 3.39 mmol) followed by Ag2O (1.18 g, 5.08 mmol) and the resulting mixture (protected from light) was stirred overnight at 40° C. The reaction mixture was filtered and the solvent was removed under reduced pressure. Purification of the residue by FC (7:3 hept-EA) gave the title compound as a yellow oil: TLC: rf (7:3 hept-EA)=0.29. LC-MS-conditions 07: tR=0.62 min, [M+H]+=176.26.
後処理
- filtrationThe reaction mixture was filtered
- customthe solvent was removed under reduced pressure
- customPurification of the residue by FC (7:3 hept-EA)
出典と根拠
- ORDレコード
- ord-5ddf421da2d54c7cb5d9b0321fe2070e
- 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…