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Ethyl chloroacetate → (5S)-5-cyclopropylmorpholin-3-one

HRID 2366353
Notes
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Reaction equation

HRID 2366353 reaction equation
[H-].[Na+].[NH2:3][C@@H:4]([CH:7]1[CH2:9][CH2:8]1)[CH2:5][OH:6].Cl[CH2:11][C:12](OCC)=[O:13]>C1(C)C=CC=CC=1>[CH:7]1([C@@H:4]2[NH:3][C:12](=[O:13])[CH2:11][O:6][CH2:5]2)[CH2:9][CH2:8]1
ParticipantsProcedureWorkupSources & evidenceReaction notes

Participants

5

Reactant 3

HCID 7751Ethyl chloroacetateHCID 24758Sodium hydrideHCID 55283785(2S)-2-amino-2-cyclopropylethan-1-ol

Product 1

HCID 58074457(5S)-5-cyclopropylmorpholin-3-oneYield 21.9%

Reagents, catalysts & solvents 1

HCID 1140TolueneSolvent3×

Procedure

To a cold, stirred suspension of sodium hydride (600 mg, 14.99 mmol) in toluene (20 mL) was added dropwise a solution of (S)-2-amino-2-cyclopropylethanol (680 mg, 6.72 mmol)) in toluene (12 mL). The reaction mixture was then allowed to warm to room temperature and a solution of ethyl chloroacetate (824 mg, 6.72 mmol) in toluene (4 mL) was added dropwise. The resulting mixture was stirred for 3 h at room temperature. The mixture was then quenched with the addition of 10 mL of 1N aq. hydrochloric acid and concentrated under vacuum. The residue was diluted with THF, dried with magnesium sulfate, concentrated under vacuum and filtered through a pad of silica gel, flushing with additional THF. The resulting filtrate was concentrated under vacuum, and the residue was further purified by flash chromatography (ISCO, 12 g silica gel column, using a 0-100% ethyl acetate in n-heptane gradient as the eluent to afford 208 mg of (S)-5-cyclopropylmorpholin-3-one as a white solid (MS: (M+H)+=142.2).

Workup

  1. stirringThe resulting mixture was stirred for 3 h at room temperature
  2. customThe mixture was then quenched with the addition of 10 mL of 1N aq. hydrochloric acid
  3. concentrationconcentrated under vacuum
  4. additionThe residue was diluted with THF
  5. dry with materialdried with magnesium sulfate
  6. concentrationconcentrated under vacuum
  7. filtrationfiltered through a pad of silica gel
  8. customflushing with additional THF
  9. concentrationThe resulting filtrate was concentrated under vacuum
  10. customthe residue was further purified by flash chromatography (ISCO, 12 g silica gel column

Sources & evidence

ORD record
ord-a4eca5776f324ce8801e418d483a4f8b
Source dataset
uspto-grants-2014_04
DOI
10.6084/m9.figshare.5104873.v1
Patent number
US08697739B2

Reaction notes

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