Sodium Azide → 2-(2-Fluoro-4-iodophenylamino)-1,5-dimethyl-6-oxo-1,6-dihydropyridine-3-carbonyl azide

HRID 1186763노트

반응식

HRID 1186763 반응식
[F:1][C:2]1[CH:7]=[C:6]([I:8])[CH:5]=[CH:4][C:3]=1[NH:9][C:10]1[N:11]([CH3:28])[C:12](=[O:27])[C:13]([CH3:26])=[CH:14][C:15]=1[C:16](ON1C(=O)CCC1=O)=[O:17].C1COCC1.CC(C)=O.[N-:38]=[N+:39]=[N-:40].[Na+]>O>[F:1][C:2]1[CH:7]=[C:6]([I:8])[CH:5]=[CH:4][C:3]=1[NH:9][C:10]1[N:11]([CH3:28])[C:12](=[O:27])[C:13]([CH3:26])=[CH:14][C:15]=1[C:16]([N:38]=[N+:39]=[N-:40])=[O:17]

참가 물질

5

반응물 3

HCID 33557Sodium AzideHCID 22559816Acetone tetrahydrofuranHCID 866645042,5-Dioxopyrrolidin-1-yl 2-(2-fluoro-4-iodophenylamino)-1,5-dimethyl-6-oxo-1,6-dihydropyridine-3-carboxylate

생성물 1

HCID 866645052-(2-Fluoro-4-iodophenylamino)-1,5-dimethyl-6-oxo-1,6-dihydropyridine-3-carbonyl azide수율 96%

시약·촉매·용매 1

HCID 962Water용매

실험 절차

A 100 ml round-bottom flask was charged with 2,5-dioxopyrrolidin-1-yl 2-(2-fluoro-4-iodophenylamino)-1,5-dimethyl-6-oxo-1,6-dihydropyridine-3-carboxylate (1.2 g, 2.40 mmol) and a mixture of THF/acetone (15 mL/30 mL). To the mixture was added NaN3 (0.52 g, 8 mmol) is previously dissolved in H2O (10 mL). The reaction mixture was stirred art room temperature for 16 hours and the organic solvents were removed under reduced pressure yielding to the desired product as a light brown solid (0.98 g, 96%).

후처리

  1. customthe organic solvents were removed under reduced pressure

출처 및 근거

ORD 기록
ord-50d26c6e1f394fc1809b93c2d7e1e113
출처 데이터셋
uspto-grants-2014_03
특허 번호
US08673919B2

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