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2-Chloroethyl chloroformate → 2-(5-Phenyl-1,2,4-oxadiazol-3-yl)morpholine hydrochloride

HRID 1896176
Notes
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Reaction equation

HRID 1896176 reaction equation
C([N:8]1[CH2:13][CH2:12][O:11][CH:10]([C:14]2[N:18]=[C:17]([C:19]3[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=3)[O:16][N:15]=2)[CH2:9]1)C1C=CC=CC=1.[Cl:25]C(OCCCl)=O>ClCCCl>[ClH:25].[C:19]1([C:17]2[O:16][N:15]=[C:14]([CH:10]3[O:11][CH2:12][CH2:13][NH:8][CH2:9]3)[N:18]=2)[CH:20]=[CH:21][CH:22]=[CH:23][CH:24]=1
ParticipantsConditionsProcedureWorkupSources & evidenceReaction notes

Participants

4

Reactant 2

HCID 123052-Chloroethyl chloroformateHCID 580978824-Benzyl-2-(5-phenyl-1,2,4-oxadiazol-3-yl)morpholine2×

Product 1

HCID 668424982-(5-Phenyl-1,2,4-oxadiazol-3-yl)morpholine hydrochloride

Reagents, catalysts & solvents 1

HCID 111,2-DichloroethaneSolvent

Conditions

Temperature
70 °C

Procedure

To a stirred solution of 4-benzyl-2-(5-phenyl-1,2,4-oxadiazol-3-yl)morpholine (intermediate 27, 900 mg, 2.80 mmol) in 1,2-dichloroethane (2.0 ml) was added chloroethyl chloroformate (0.46 ml, 4.20 mmol), and the reaction mixture was stirred at 70° C. for 4 hours. The reaction mixture was concentrated in vacuo. After removal of the solvent, the residue was dissolved in methanol (2.0 ml), and the solution was stirred under reflux for one hour. When the reaction was complete (checked by thin layer chromatography), the reaction mixture was concentrated in vacuo. The resulting 2-(5-phenyl-[1,2,4]oxadiazol-3-yl)-morpholine hydrochloride (intermediate 28) was used for next reaction without further purification.

Workup

  1. concentrationThe reaction mixture was concentrated in vacuo
  2. customAfter removal of the solvent
  3. dissolutionthe residue was dissolved in methanol (2.0 ml)
  4. stirringthe solution was stirred
  5. temperatureunder reflux for one hour
  6. concentrationthe reaction mixture was concentrated in vacuo
  7. customThe resulting 2-(5-phenyl-[1,2,4]oxadiazol-3-yl)-morpholine hydrochloride (intermediate 28) was used for next reaction without further purification

Sources & evidence

ORD record
ord-f12cdea224d1460d9fa98a09d1e847d5
Source dataset
uspto-grants-2013_08
DOI
10.6084/m9.figshare.5104873.v1
Patent number
US08518939B2

Reaction notes

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On this pageParticipantsConditionsProcedureWorkupSources & evidenceReaction notes