Trifluoroacetic acid → (Piperidin-4-yl)(thiophen-2-yl)methanone
反応式
[S:1]1[CH:5]=[CH:4][CH:3]=[C:2]1[C:6]([CH:8]1[CH2:13][CH2:12][N:11](C(OC(C)(C)C)=O)[CH2:10][CH2:9]1)=[O:7].FC(F)(F)C(O)=O>C(OCC)C>[S:1]1[CH:5]=[CH:4][CH:3]=[C:2]1[C:6]([CH:8]1[CH2:9][CH2:10][NH:11][CH2:12][CH2:13]1)=[O:7]参加物
4
実験手順
Mix 4-[(thiophene-2-yl)carbonyl]-1-piperidinecarboxylic acid, 1,1-dimethylethyl ester (12.9 g, 43.67 mmol) and trifluoroacetic acid (80 mL) and stir at room temperature for 2 hours. Cool in an ice/water bath and dilute with ethyl ether. Collect the resulting solid by filtration, wash with ethyl acetate and recrystallize (methanol/ethyl ether) to give the title compound as an off-white solid; mp 186°-187° C.
後処理
- temperatureCool in an ice/water bath
- customCollect the resulting solid
- filtrationby filtration
- washwash with ethyl acetate
- customrecrystallize (methanol/ethyl ether)
出典と根拠
- ORDレコード
- ord-4810d2772701441b87864a626c281b16
- 出典データセット
- uspto-grants-1998_04
- 特許番号
- US05739150
反応ノート
読み込み中…