Sodium Carbonate → HCID 20132570, compound

HRID 845278Notes

Reaction equation

HRID 845278 reaction equation
[CH2:1]([N:8]([CH2:10][C:11]1[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=1)[OH:9])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[C:17](=O)([O-])[O-].[Na+].[Na+].[I-].C[CH:25]=[N+:26]=[CH:27]C>C(Cl)Cl>[CH2:10]([N:8]([CH2:1][C:2]1[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=1)[O:9][CH2:25][N:26]([CH3:27])[CH3:17])[C:11]1[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=1

Participants

5

Reactant 3

HCID 10340Sodium CarbonateHCID 69297DibenzylhydroxylamineHCID 21892197N,N-dimethylmethyleneammoniumiodide

Product 1

HCID 20132570HCID 20132570, compound

Reagents, catalysts & solvents 1

HCID 6344DichloromethaneSolvent

Procedure

A mixture of 4.86 g of dibenzylhydroxylamine, 2.42 g of anhydrous sodium carbonate and 4.22 g of N,N-dimethylmethyleneammoniumiodide in 50 ml of methylene chloride is stirred at room temperature under N2 for 48 hrs. After removal of the insoluble inorganic residue by filtration, the solution is concentrated under reduced pressure. The resulting residue is treated with heptane to extract the product. Removal of the combined heptane extracts affords the product as a thick oil.

Workup

  1. customAfter removal of the insoluble inorganic residue
  2. filtrationby filtration
  3. concentrationthe solution is concentrated under reduced pressure
  4. additionThe resulting residue is treated with heptane
  5. extractionto extract the product
  6. customRemoval of the combined heptane

Sources & evidence

ORD record
ord-df4f981768324f569b88fb0a4038dc9d
Source dataset
uspto-grants-1988_07
Patent number
US04757102

Reaction notes

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