Sulfuric acid magnesium salt (1:1) → HCID 23446882、化合物

HRID 1841634ノート

反応式

HRID 1841634 の反応式
[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

参加物

5

反応物 3

HCID 24083Sulfuric acid magnesium salt (1:1)HCID 13345321HCID 13345321、化合物HCID 23446892HCID 23446892、化合物

生成物 1

HCID 23446882HCID 23446882、化合物

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

反応条件

温度
170 °C

実験手順

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.

後処理

  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.

出典と根拠

ORDレコード
ord-3d4e2b211cc54807b9cf22ee1050d50c
出典データセット
uspto-grants-2004_01
特許番号
US06683213B1

反応ノート

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