Methyl iodide → HCID 22325143, compound

HRID 496056Notes

Reaction equation

HRID 496056 reaction equation
[H-].[Na+].[CH3:3][O:4][C:5]([NH:7][C:8]1([C:11]([O:13][CH3:14])=[O:12])[CH2:10][CH2:9]1)=[O:6].[CH3:15]I>CN(C)C=O>[CH3:3][O:4][C:5]([N:7]([CH3:15])[C:8]1([C:11]([O:13][CH3:14])=[O:12])[CH2:10][CH2:9]1)=[O:6]

Participants

5

Reactant 3

HCID 6328Methyl iodideHCID 24758Sodium hydrideHCID 13134738HCID 13134738, compound

Product 1

HCID 22325143HCID 22325143, compound

Reagents, catalysts & solvents 1

HCID 6228DimethylformamideSolvent

Procedure

24.7 g of sodium hydride are added, in fractions, to a solution, cooled to 5° C., of 99.7 g of the compound obtained in Step 2 in 1.7 liters of anhydrous dimethylformamide. After 15 minutes at 5° C. and then 3 hours at ambient temperature, 38.2 ml of methyl iodide are added dropwise. After reacting for 20 hours, the mixture is evaporated. The residue is taken up in ether and then treated in conventional manner. Chromatography over silica gel (dichloromethane) allows the expected product to be isolated.

Workup

  1. waitAfter reacting for 20 hours
  2. customthe mixture is evaporated
  3. additiontreated in conventional manner
  4. customto be isolated

Sources & evidence

ORD record
ord-b9f285fd15aa4d5e8639242a8e9bb248
Source dataset
uspto-grants-2005_09
Patent number
US06943184B2

Reaction notes

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