2-Methylene4-morpholin-4-yl-4-oxo-butyric acid → HCID 22053968, compound
Reaction equation
[N:1]1([C:7](=[O:14])[CH2:8][C:9](=[CH2:13])[C:10]([OH:12])=[O:11])[CH2:6][CH2:5][O:4][CH2:3][CH2:2]1.[C:15]([O-:18])(=[S:17])[CH3:16].[K+]>CN(C=O)C>[C:15]([S:17][CH2:13][CH:9]([CH2:8][C:7]([N:1]1[CH2:2][CH2:3][O:4][CH2:5][CH2:6]1)=[O:14])[C:10]([OH:12])=[O:11])(=[O:18])[CH3:16]Participants
4
Reactant 2
Product 1
Reagents, catalysts & solvents 1
Procedure
2-(2-morpholin-4-yl-2-oxo-ethyl)-acrylic acid (55.19 g, 277.0 mmol) was dissolved in 120 mL DMF and set to stir at room temperature. Potassium thioacetate (25 g, 219.0 mmol) was added in one portion, and the reaction mixture was allowed to stir at ambient temperature for 20 hours. Upon completion (LCMS), DMF was removed by vacuum under reduced pressure. Crude Yield: 75 g. Percent Purity (LCMS): 40%. The crude product was used without further purification.
Workup
- stirringto stir at ambient temperature for 20 hours
- customUpon completion (LCMS), DMF was removed by vacuum under reduced pressure
- customThe crude product was used without further purification
Sources & evidence
- ORD record
- ord-00f387b73a2e4e428afe70a764e94ede
- Source dataset
- uspto-grants-2006_06
- Patent number
- US07064123B1
Reaction notes
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