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

HRID 992851ノート

反応式

HRID 992851 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 A4 were added to 2.9 g (17.7 mmol) of 6-methylpyridine-2,3-dicarboxylic anhydride and, after heating to 170° C., stirred as a melt for a total of 8 h. After cooling, the residue was taken up in methylene chloride, and activated carbon and magnesium sulfate were added. The mixture was filtered off with suction and chromatographed on silica gel giving, after concentration, 1.3 g (24.4% of theory) of the title compound as beige crystals of m.p. 173-176° C.

後処理

  1. temperatureAfter cooling
  2. filtrationThe mixture was filtered off with suction
  3. customchromatographed on silica gel giving
  4. concentrationafter concentration, 1.3 g (24.4% of theory) of the title compound as beige crystals of m.p. 173-176° C.

出典と根拠

ORDレコード
ord-18a3936b51644059b060c008179a7973
出典データセット
uspto-grants-2002_10
特許番号
US06472349B1

反応ノート

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