HCID 58857936, compound → HCID 54692332, compound

HRID 2114815Notes

Reaction equation

HRID 2114815 reaction equation
CO[C:3]1[CH2:8][CH2:7][N:6]([CH3:9])[C:5](=[O:10])[C:4]=1[C:11]([O:13]CC)=O.[Cl:16][C:17]1[CH:18]=[C:19]([CH:28]=[CH:29][C:30]=1[F:31])[CH2:20][N:21]1[CH2:26][CH2:25][NH:24][CH2:23][C:22]1=[O:27]>C(O)CO.CO>[Cl:16][C:17]1[CH:18]=[C:19]([CH:28]=[CH:29][C:30]=1[F:31])[CH2:20][N:21]1[CH2:26][CH2:25][N:24]2[C:3]3[CH2:8][CH2:7][N:6]([CH3:9])[C:5](=[O:10])[C:4]=3[C:11]([OH:13])=[C:23]2[C:22]1=[O:27]

Participants

5

Reactant 2

HCID 58857936HCID 58857936, compoundHCID 69145692HCID 69145692, compound

Product 1

HCID 54692332HCID 54692332, compound

Reagents, catalysts & solvents 2

HCID 174Ethylene GlycolSolventHCID 887MethanolSolvent

Conditions

Temperature
250 °C

Procedure

A mixture of ethyl 4-methoxy-1-methyl-2-oxo-1,2,5,6-tetrahydropyridine-3-carboxylate (0.27 g, 1.27 mmol) and 1-(3-chloro-4-fluorobenzyl)piperazin-2-one (0.92 g, 3.80 mmol) in ethylene glycol (2.5 mL) was heated in a sealed tube at 250° C. in a microwave reactor for 20 minutes with stirring. The resultant solution was diluted with methanol (2.5 mL) and cooled to 0° C. The white solid precipitate was filtered, washed successively with cold methanol and diethyl ether, and then dried under vacuum to provide the title compound.

Workup

  1. temperaturecooled to 0° C
  2. filtrationThe white solid precipitate was filtered
  3. washwashed successively with cold methanol and diethyl ether
  4. customdried under vacuum

Sources & evidence

ORD record
ord-ebbba639bc7c492c9073915fd44797ff
Source dataset
uspto-grants-2008_10
Patent number
US07435735B2

Reaction notes

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