Sulfuric acid magnesium salt (1:1) → HCID 23446882, compound

HRID 1841634Notes

Reaction equation

HRID 1841634 reaction equation
[NH2:1][C:2]1[C:9]([Cl:10])=[CH:8][CH:7]=[C:6]([CH3:11])[C:3]=1[C:4]#[N:5].[CH3:12][C:13]1[N:18]=[C:17]2[C:19]([O:21][C:22](=O)[C:16]2=[CH:15][CH:14]=1)=[O:20].S([O-])([O-])(=O)=O.[Mg+2]>C(Cl)Cl>[Cl:10][C:9]1[C:2]([N:1]2[C:22](=[O:21])[C:16]3[C:17](=[N:18][C:13]([CH3:12])=[CH:14][CH:15]=3)[C:19]2=[O:20])=[C:3]([C:4]#[N:5])[C:6]([CH3:11])=[CH:7][CH:8]=1

Participants

5

Reactant 3

HCID 24083Sulfuric acid magnesium salt (1:1)HCID 13345321HCID 13345321, compoundHCID 23446892HCID 23446892, compound

Product 1

HCID 23446882HCID 23446882, compound

Reagents, catalysts & solvents 1

HCID 6344DichloromethaneSolvent

Conditions

Temperature
170 °C

Procedure

3.1 g (18.61 mmol) of the compound from example 4 were added to 2.9 g (17.7 mmol) of 6-methylpyridine-2,3-dicarboxylic anhydride and, with warming to 170° C., the mixture was stirred for a total of 8 h as a melt. After cooling, the residue was taken up in methylene chloride, and the solution was treated with active carbon and magnesium sulfate. After filtering off with suction, the filtrate was chromatographed on silica gel, 1.3 g (24.4% of theory) of the title compound being obtained after concentration as beige crystals of m.p. 173-176° C.

Workup

  1. temperatureAfter cooling
  2. filtrationAfter filtering off with suction
  3. customthe filtrate was chromatographed on silica gel, 1.3 g (24.4% of theory) of the title compound
  4. custombeing obtained
  5. concentrationafter concentration as beige crystals of m.p. 173-176° C.

Sources & evidence

ORD record
ord-3d4e2b211cc54807b9cf22ee1050d50c
Source dataset
uspto-grants-2004_01
Patent number
US06683213B1

Reaction notes

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