Water → HCID 59299383, compound
Reaction equation
[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]1Participants
5
Reactant 3
Product 1
Reagents, catalysts & solvents 1
Procedure
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).
Workup
- 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
Sources & evidence
- ORD record
- ord-88ed05f8e9f4480eba70c5572f6e9684
- Source dataset
- uspto-grants-2010_05
- Patent number
- US07713979B2
Reaction notes
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