Water → HCID 59299383、化合物
反応式
[H-].[Na+].Cl[CH2:4][CH2:5][CH2:6][C:7]([NH:9][N:10]1[CH2:15][CH2:14][CH2:13][CH2:12][CH2:11]1)=[O:8].O>C1COCC1>[N:10]1([N:9]2[CH2:4][CH2:5][CH2:6][C:7]2=[O:8])[CH2:15][CH2:14][CH2:13][CH2:12][CH2:11]1参加物
5
実験手順
Add NaH (1 g, 25 mmol) into 4-chloro-N-piperidin-1-yl-butyramide (Preparation 10) (3.2 g, 16 mmol) in THF (100 mL) and stir for 1 hour. Add the reaction mixture into water and extract with ethyl acetate (100 mL). Wash the organic layer with brine (20 mL), dry with magnesium sulfate, filter and evaporate solvent under reduced pressure. Purify the residue by column chromatography to give the title product (2 g, 76%) as yellow oil: Mass spectrum (ion spray): m/z=169.1 (M+H).
後処理
- extractionextract with ethyl acetate (100 mL)
- washWash the organic layer with brine (20 mL)
- dry with materialdry with magnesium sulfate
- filtrationfilter
- customevaporate solvent under reduced pressure
- customPurify the residue by column chromatography
出典と根拠
- ORDレコード
- ord-88ed05f8e9f4480eba70c5572f6e9684
- 出典データセット
- uspto-grants-2010_05
- 特許番号
- US07713979B2
反応ノート
読み込み中…