3-Methylpiperidine → HCID 178426353, compound

HRID 414456Notes

Reaction equation

HRID 414456 reaction equation
Cl[C:2]1[N:7]=[C:6]([C:8]([NH:10][C:11]2[NH:15][N:14]=[N:13][N:12]=2)=[O:9])[CH:5]=[N:4][CH:3]=1.[CH3:16][CH:17]1[CH2:22][CH2:21][CH2:20][NH:19][CH2:18]1>C1C=CC=CC=1>[CH3:16][CH:17]1[CH2:22][CH2:21][CH2:20][N:19]([C:2]2[N:7]=[C:6]([C:8]([NH:10][C:11]3[NH:15][N:14]=[N:13][N:12]=3)=[O:9])[CH:5]=[N:4][CH:3]=2)[CH2:18]1

Participants

4

Reactant 2

HCID 790813-MethylpiperidineHCID 178522716HCID 178522716, compound

Product 1

HCID 178426353HCID 178426353, compound

Reagents, catalysts & solvents 1

HCID 241BenzeneSolvent

Procedure

To a suspension of 1.13 g of 6-chloro-N-(1H-5-tetrazolyl)pyrazine-2-carboxamide in 20 ml of benzene, 2.94 ml of 3-methylpiperidine was added, and the mixture was refluxed for 6 hours. The reation mixture was evaporated, ethanol was added to the residue, and then the ethanol solution was adjusted with ethanolic hydrogen chloride to pH 3. The precipitate was collected by filtration, and recrystalized from a mixture of dimethylsulfoxide and methanol affording 0.81 g of the desired compound as pale yellow columns, m.p. 236.5°-238.5 ° C.

Workup

  1. additionwas added
  2. temperaturethe mixture was refluxed for 6 hours
  3. customThe reation mixture was evaporated
  4. additionethanol was added to the residue
  5. filtrationThe precipitate was collected by filtration
  6. customrecrystalized from a mixture of dimethylsulfoxide and methanol affording 0.81 g of the desired compound as pale yellow columns, m.p. 236.5°-238.5 ° C.

Sources & evidence

ORD record
ord-8d8ea68ecb5a4f2689781b9b3bb0b2fb
Source dataset
uspto-grants-1988_12
Patent number
US04792547

Reaction notes

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