m-Chloroperbenzoic acid → HCID 9856230, compound

HRID 354237Notes

Reaction equation

HRID 354237 reaction equation
[C:1]1(=[C:7]([C:10]2[CH:15]=[CH:14][C:13]([O:16][CH3:17])=[CH:12][CH:11]=2)[C:8]#[N:9])[CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]1.ClC1C=CC=C(C(OO)=[O:26])C=1>ClCCl>[CH3:17][O:16][C:13]1[CH:14]=[CH:15][C:10]([C:7]2([C:8]#[N:9])[C:1]3([CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]3)[O:26]2)=[CH:11][CH:12]=1

Participants

4

Reactant 2

HCID 70297m-Chloroperbenzoic acidHCID 1286244580526-53-0

Product 1

HCID 9856230HCID 9856230, compound

Reagents, catalysts & solvents 1

HCID 6344DichloromethaneSolvent

Procedure

2.0 g of the product from Stage 1 was refluxed for 8 hours with 2.0 g of m-chloro-perbenzoic acid, in dichloromethane. The reaction mixture was cooled to room temperature and filtered to remove precipitated m-chloro-perbenzoic acid. The filtrate was washed with saturated sodium bicarbonate solution, and the dichloromethane layer was then dried over sodium sulphate. The solvent was distilled under reduced pressure, and the residue purified by column chloromatography using a hexane:benzene (8:2) mixture as the mobile phase.

Workup

  1. filtrationfiltered
  2. customto remove
  3. customprecipitated m-chloro-perbenzoic acid
  4. washThe filtrate was washed with saturated sodium bicarbonate solution
  5. dry with materialthe dichloromethane layer was then dried over sodium sulphate
  6. distillationThe solvent was distilled under reduced pressure
  7. customthe residue purified by column chloromatography

Sources & evidence

ORD record
ord-ef92446f3e6542b3aa4d5f5eaf338c98
Source dataset
uspto-grants-2004_06
Patent number
US06756502B2

Reaction notes

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