HCID 70225330, compound → HCID 70227863, compound

HRID 324422Notes

Reaction equation

HRID 324422 reaction equation
O[C:2]1([C:18]2[C:19]([O:29]C(C)(C)C)=[N:20][C:21]([O:24]C(C)(C)C)=[N:22][CH:23]=2)[C:11]2[O:10][C:9]([CH3:12])=[N:8][C:7]=2[CH2:6][CH2:5][C:4]2[CH:13]=[C:14]([CH3:17])[CH:15]=[CH:16][C:3]1=2>C(O)(=O)C>[CH3:12][C:9]1[O:10][C:11]2[CH:2]([C:18]3[C:19](=[O:29])[NH:20][C:21](=[O:24])[NH:22][CH:23]=3)[C:3]3[CH:16]=[CH:15][C:14]([CH3:17])=[CH:13][C:4]=3[CH:5]=[CH:6][C:7]=2[N:8]=1

Participants

3

Reactant 1

HCID 70225330HCID 70225330, compound

Product 1

HCID 70227863HCID 70227863, compound

Reagents, catalysts & solvents 1

HCID 176Acetic AcidSolvent2×

Conditions

Temperature
100 °C

Procedure

A solution of the product from step (vi) (5.7 g) in acetic acid (20 ml) was added dropwise over 5 min to acetic acid heated at 100° C. The mixture was heated for a further 3 hours at 100° C., the solvent removed under reduced pressure and azeotroped with toluene. Purification was by chromatography eluting with 5% methanol in dichloromethane.

Workup

  1. temperatureThe mixture was heated for a further 3 hours at 100° C.
  2. customthe solvent removed under reduced pressure
  3. customazeotroped with toluene
  4. customPurification
  5. washeluting with 5% methanol in dichloromethane

Sources & evidence

ORD record
ord-49bf0177f1f54b4f90414c26c13c4762
Source dataset
uspto-grants-2001_04
Patent number
US06218376B1

Reaction notes

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