Lithium Hydroxide → HCID 66756006, compound

HRID 1642140Notes

Reaction equation

HRID 1642140 reaction equation
[OH-].[Li+].[Cl:3][C:4]1[CH:9]=[C:8]([Cl:10])[CH:7]=[CH:6][C:5]=1[S:11]([N:14]1[CH2:19][CH2:18][NH:17][C:16](=[O:20])[CH:15]1[CH2:21][C:22]([O:24]CC)=[O:23])(=[O:13])=[O:12]>CO.O>[Cl:3][C:4]1[CH:9]=[C:8]([Cl:10])[CH:7]=[CH:6][C:5]=1[S:11]([N:14]1[CH2:19][CH2:18][NH:17][C:16](=[O:20])[CH:15]1[CH2:21][C:22]([OH:24])=[O:23])(=[O:13])=[O:12]

Participants

5

Reactant 2

HCID 3939Lithium HydroxideHCID 3767271HCID 3767271, compound

Product 1

HCID 66756006HCID 66756006, compound

Reagents, catalysts & solvents 2

HCID 887MethanolSolventHCID 962WaterSolvent

Procedure

Lithium hydroxide (0.92 mg, 21.9 mmol) was added to a cooled solution of ethyl 2-(1-(2,4-dichlorophenylsulfonyl)-3-oxopiperazin-2-yl)acetate (2.7 g, 7.3 mmol) in methanol (25 ml) and water (6 ml), and stirring was carried out for 16 h at room temperature (TLC monitoring). The solvent was removed using a rotary evaporator and the residue was taken up in water. The aqueous phase was washed with diethyl ether and acidified with HCl, and the product was extracted with ethyl acetate. The organic phase was then washed with saturated NaCl solution. The organic phase was dried over sodium sulfate and concentrated to dryness.

Workup

  1. customThe solvent was removed
  2. customa rotary evaporator
  3. washThe aqueous phase was washed with diethyl ether
  4. extractionthe product was extracted with ethyl acetate
  5. washThe organic phase was then washed with saturated NaCl solution
  6. dry with materialThe organic phase was dried over sodium sulfate
  7. concentrationconcentrated to dryness

Sources & evidence

ORD record
ord-a830e8ac4c3b472a91f642206594d231
Source dataset
uspto-grants-2012_02
Patent number
US08119633B2

Reaction notes

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