2-Methylene4-morpholin-4-yl-4-oxo-butyric acid → HCID 22053968, compound

HRID 1830152Notes

Reaction equation

HRID 1830152 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

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

  1. stirringto stir at ambient temperature for 20 hours
  2. customUpon completion (LCMS), DMF was removed by vacuum under reduced pressure
  3. 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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