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

HRID 1841634노트

반응식

HRID 1841634 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

반응 조건

온도
170 °C

실험 절차

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.

후처리

  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.

출처 및 근거

ORD 기록
ord-3d4e2b211cc54807b9cf22ee1050d50c
출처 데이터셋
uspto-grants-2004_01
특허 번호
US06683213B1

반응 노트

불러오는 중…