Dichloromethane → HCID 10758665, compound

HRID 565103Notes

Reaction equation

HRID 565103 reaction equation
CS[C:3]1[CH:8]=[CH:7][C:6]([C:9]2[CH2:13][CH2:12][C:11](=[O:14])[C:10]=2[O:15][C:16]2[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=2)=[CH:5][CH:4]=1.O[O:23][S:24]([O-:26])=O.[K+].Cl[CH2:29]Cl>CO.O>[CH3:29][S:24]([C:3]1[CH:4]=[CH:5][C:6]([C:9]2[CH2:13][CH2:12][C:11](=[O:14])[C:10]=2[O:15][C:16]2[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=2)=[CH:7][CH:8]=1)(=[O:26])=[O:23]

Participants

6

Reactant 3

HCID 6344DichloromethaneHCID 22114259HCID 22114259, compoundHCID 23707502Potassium hydroxy sulfite

Product 1

HCID 10758665HCID 10758665, compound

Reagents, catalysts & solvents 2

HCID 887MethanolSolventHCID 962WaterSolvent2×

Procedure

To the compound obtained in Step 2 (60 mg) in dichloromethane (4.5 mL) and methanol (2.4 mL) was added Oxone ® (450 mg) in water (1 mL) and the reaction mixture was stirred for 1 h. Water was added to the mixture which was then extracted with dichloromethane, the organic layers were combined and dried over MgSO4, filtered and the solvent evaporated under vacuum. Purification by silica gel chromatograohy afforded the title compound.

Workup

  1. extractionwas then extracted with dichloromethane
  2. dry with materialdried over MgSO4
  3. filtrationfiltered
  4. customthe solvent evaporated under vacuum
  5. customPurification by silica gel chromatograohy

Sources & evidence

ORD record
ord-22ab350402a64ee2b710830b99d6c699
Source dataset
uspto-grants-2001_01
Patent number
US06169188A

Reaction notes

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