HCID 67641045, compound → HCID 18916198, compound

HRID 1290601Notes

Reaction equation

HRID 1290601 reaction equation
[NH2:1][C:2](=[N:21][C:22]1[CH:33]=[CH:32][C:25]([C:26]([O:28]CC=C)=[O:27])=[CH:24][CH:23]=1)[C:3]1[CH:8]=[CH:7][C:6]([O:9][CH3:10])=[C:5]([C:11]23[CH2:20]C4CC(CC(C4)[CH2:12]2)[CH2:18]3)[CH:4]=1>CO>[NH2:1][C:2](=[N:21][C:22]1[CH:23]=[CH:24][C:25]([C:26]([OH:28])=[O:27])=[CH:32][CH:33]=1)[C:3]1[CH:8]=[CH:7][C:6]([O:9][CH3:10])=[C:5]([C:11]([CH3:20])([CH3:12])[CH3:18])[CH:4]=1

Participants

3

Reactant 1

HCID 67641045HCID 67641045, compound

Product 1

HCID 18916198HCID 18916198, compoundYield 78%

Reagents, catalysts & solvents 1

HCID 887MethanolSolvent2×

Procedure

In a round bottom flask, there are introduced 300 mg (0.82 mmole) of the derivative obtained above in (c), 180 mg (4.5 mmoles) of soda and 10 ml of methanol. After 24 hours of reaction at reflux of the methanol, the mixture is evaporated and the remainder is taken up in water. The reaction mixture is neutralized to pH 5-6 by acetic acid. The resulting precipitate is filtered, washed with demineralized water and then dried for 48 hours at 80° C. 210 mg (78%) of the expected acid whose melting point is 170°-172° C. are obtained

Workup

  1. additionIn a round bottom flask, there are introduced 300 mg (0.82 mmole) of the
  2. customAfter 24 hours of reaction
  3. customthe mixture is evaporated
  4. filtrationThe resulting precipitate is filtered
  5. washwashed with demineralized water
  6. customdried for 48 hours at 80° C

Sources & evidence

ORD record
ord-199f00fb446440f9b649d22bb0216ffa
Source dataset
uspto-grants-1998_05
Patent number
US05753239

Reaction notes

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