HCID 22401698, compound → HCID 22401694, compound

HRID 260517Notes

Reaction equation

HRID 260517 reaction equation
C([O:5][C:6]([CH2:8][N:9]1[CH:17]=[C:16]2[C:11]([N:12]=[C:13]3[S:21][CH2:20][CH2:19][N:14]3[C:15]2=[O:18])=[N:10]1)=[O:7])(C)(C)C>FC(F)(F)C(O)=O>[C:6]([CH2:8][N:9]1[CH:17]=[C:16]2[C:11]([N:12]=[C:13]3[S:21][CH2:20][CH2:19][N:14]3[C:15]2=[O:18])=[N:10]1)([OH:7])=[O:5]

Participants

3

Reactant 1

HCID 22401698HCID 22401698, compound

Product 1

HCID 22401694HCID 22401694, compoundYield 70%

Reagents, catalysts & solvents 1

HCID 6422Trifluoroacetic acidSolvent

Procedure

In 30 ml of trifluoroacetic acid was dissolved 0.95 g (3.08 mmol) of Compound 35 prepared in Example 26, followed by heating under reflux for one hour. After evaporation of the solvent, water was added to the residue. The precipitated crystals were collected by filtration, followed by washing with water to give 0.54 g (70%) of Compound 37. The compound was recrystallized from dimethylformamide/water for purification.

Workup

  1. temperatureby heating
  2. temperatureunder reflux for one hour
  3. customAfter evaporation of the solvent, water
  4. additionwas added to the residue
  5. filtrationThe precipitated crystals were collected by filtration
  6. washby washing with water

Sources & evidence

ORD record
ord-015b4feeb3dd4322bc41c289d5883101
Source dataset
uspto-grants-1996_06
Patent number
US05527908

Reaction notes

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