Water → HCID 20083100, compound

HRID 1609100Notes

Reaction equation

HRID 1609100 reaction equation
[F:1][C:2]1[C:11]([F:12])=[C:10]([F:13])[C:9]2[C:14](=[O:22])[C:15]([C:17]([O:19][CH2:20][CH3:21])=[O:18])=[CH:16][N:7]3[C:8]=2[C:3]=1[CH:4](C(O)=O)[CH2:5][N:6]3[CH3:23].O>CN1CCCC1=O>[F:1][C:2]1[C:11]([F:12])=[C:10]([F:13])[C:9]2[C:14](=[O:22])[CH:15]([C:17]([O:19][CH2:20][CH3:21])=[O:18])[CH2:16][N:7]3[C:8]=2[C:3]=1[CH2:4][CH2:5][N:6]3[CH3:23]

Participants

4

Reactant 2

HCID 962WaterHCID 20083105HCID 20083105, compound

Product 1

HCID 20083100HCID 20083100, compoundYield 49%

Reagents, catalysts & solvents 1

HCID 13387N-methyl-2-pyrrolidoneSolvent

Conditions

Temperature
160 °C

Procedure

300 mg of the compound (197) obtained in Example 68 was dissolved in 6 ml of N-methylpyrrolidone, and the solution was heated at 160° C. for 3 hours. After air-cooling, the water was added to the reaction solution, and the solution was extracted with chloroform three times. After drying over magnesium sulfate, the solvent was removed by distillation. The residue was separated by column chromatography (silica gel, eluent solvent; chloroform) to obtain 128 mg of the subject compound (198) in a 49% yield.

Workup

  1. temperatureAfter air-cooling
  2. extractionthe solution was extracted with chloroform three times
  3. dry with materialAfter drying over magnesium sulfate
  4. customthe solvent was removed by distillation
  5. customThe residue was separated by column chromatography (silica gel, eluent solvent; chloroform)

Sources & evidence

ORD record
ord-9ee8769331ec4b46ab167679e996b6a8
Source dataset
uspto-grants-1995_03
Patent number
US05399553

Reaction notes

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