HCID 178420617, compound → HCID 178511438, compound

HRID 1872016Notes

Reaction equation

HRID 1872016 reaction equation
[NH2+]1CCCC1.CC(C)(OC([NH:12][CH2:13][C:14]([NH:16][C:17]1[NH:21][N:20]=[N:19][N:18]=1)=[O:15])=O)C>C(OCC)(=O)C>[NH2:12][CH2:13][C:14]([NH:16][C:17]1[NH:21][N:20]=[N:19][N:18]=1)=[O:15]

Participants

3

Reactant 1

HCID 178420617HCID 178420617, compound

Product 1

HCID 178511438HCID 178511438, compound

Reagents, catalysts & solvents 1

HCID 8857Ethyl AcetateSolvent

Procedure

The product of step (i) (1.4 g) was slurried in ethyl acetate, washed with 1N HCl and filtered. The filtrate was washed with water, dried (MgSO4) and evaporated. The residue was dissolved in dichloromethane (50 ml) and trifluoroacetic acid (8 ml) and stirred at room temperature for 2 hours. The mixture was evaporated. The residue was azeotroped with toluene and triturated with isohexane. The product was collected by filtration. Yield 0.45 g.

Workup

  1. washwashed with 1N HCl
  2. filtrationfiltered
  3. washThe filtrate was washed with water
  4. dry with materialdried (MgSO4)
  5. customevaporated
  6. dissolutionThe residue was dissolved in dichloromethane (50 ml)
  7. customThe mixture was evaporated
  8. customThe residue was azeotroped with toluene
  9. customtriturated with isohexane
  10. filtrationThe product was collected by filtration

Sources & evidence

ORD record
ord-3263381dcef64036a069a50300a1ca7d
Source dataset
uspto-grants-2000_08
Patent number
US06107297

Reaction notes

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