Ethanol → Ethyl 3-methyl-1H-pyrazole-1-acetate
反応式
[CH3:1][C:2]1[CH:6]=[CH:5][N:4]([CH2:7][C:8]([OH:10])=[O:9])[N:3]=1.OS(O)(=O)=O.[CH3:16][CH2:17]O>C(Cl)Cl>[CH3:1][C:2]1[CH:6]=[CH:5][N:4]([CH2:7][C:8]([O:10][CH2:16][CH3:17])=[O:9])[N:3]=1参加物
5
反応条件
- 温度
- 80 °C
実験手順
A suspension of (3-methyl-1H-pyrazol-1-yl)acetic acid (200 mg) and H2SO4 (0.1 mL) in EtOH (2 mL) was stirred at 80° C. for 4 h. After cooling down, the reaction mixture was diluted with DCM and washed with sat. Na2CO3, water and brine. The aq. layers were extracted with DCM, the combined org. layers were dried (MgSO4), filtered off and evaporated in vacuo to afford ethyl 2-(3-methyl-1H-pyrazol-1-yl)acetate (101 mg, colourless liquid). LC-MS (B): tR=0.57 min; [M+H]+: 169.01.
後処理
- temperatureAfter cooling down
- washwashed with sat. Na2CO3, water and brine
- extractionThe aq. layers were extracted with DCM
- dry with materiallayers were dried (MgSO4)
- filtrationfiltered off
- customevaporated in vacuo
出典と根拠
- ORDレコード
- ord-e6189fb7faca414499d065a297922990
- 出典データセット
- uspto-grants-2016_02
- 特許番号
- US09266876B2
反応ノート
読み込み中…