Oxonium, trimethyl-, tetrafluoroborate(1-) (1:1) → methyl 5-fluoro-2-methyl-2H-indazole-4-carboxylate

HRID 1639778노트

반응식

HRID 1639778 반응식
[F:1][C:2]1[CH:10]=[CH:9][C:8]2[C:4](=[CH:5][NH:6][N:7]=2)[C:3]=1[C:11]([O:13][CH3:14])=[O:12].F[B-](F)(F)F.[CH3:20][O+](C)C>C(OCC)(=O)C.O>[F:1][C:2]1[CH:10]=[CH:9][C:8]2[C:4](=[CH:5][N:6]([CH3:20])[N:7]=2)[C:3]=1[C:11]([O:13][CH3:14])=[O:12]

참가 물질

5

반응물 2

HCID 2735153Oxonium, trimethyl-, tetrafluoroborate(1-) (1:1)HCID 178498690HCID 178498690, 화합물

생성물 1

HCID 59334518methyl 5-fluoro-2-methyl-2H-indazole-4-carboxylate수율 85%

시약·촉매·용매 2

HCID 962Water용매HCID 8857Ethyl Acetate용매

실험 절차

To a solution of methyl 5-fluoro-2H-indazole-4-carboxylate (4.50 g, 23.2 mmol) in ethyl acetate (93 mL) was 25 added trimethyloxonium tetrafluoroborate (4.46 g, 30.1 mmol) at room temperature, and the mixture was stirred for 5 hr. The reaction solution was diluted with water, and the mixture was extracted with ethyl acetate. The extract was dried over anhydrous sodium sulfate and the solvent was evaporated under reduced pressure. The residue was purified by flash silica gel column chromatography (ethyl acetate/hexane=1/2) to give the title compound (4.10 g, yield 85%).

후처리

  1. customat room temperature
  2. extractionthe mixture was extracted with ethyl acetate
  3. dry with materialThe extract was dried over anhydrous sodium sulfate
  4. customthe solvent was evaporated under reduced pressure
  5. customThe residue was purified by flash silica gel column chromatography (ethyl acetate/hexane=1/2)

출처 및 근거

ORD 기록
ord-41f5b6be4f73490db99924fd3064f90f
출처 데이터셋
uspto-grants-2012_02
특허 번호
US08110585B2

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