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

HRID 992851노트

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HRID 992851 반응식
[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

참가 물질

5

반응물 3

HCID 24083Sulfuric acid magnesium salt (1:1)HCID 13345321HCID 13345321, 화합물HCID 23446892HCID 23446892, 화합물

생성물 1

HCID 23446882HCID 23446882, 화합물

시약·촉매·용매 1

HCID 6344Dichloromethane용매

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온도
170 °C

실험 절차

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.

후처리

  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.

출처 및 근거

ORD 기록
ord-18a3936b51644059b060c008179a7973
출처 데이터셋
uspto-grants-2002_10
특허 번호
US06472349B1

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