Potassium tert-butoxide → HCID 178498690, 화합물

HRID 1639777노트

반응식

HRID 1639777 반응식
C(S[N:6]=[N:7][C:8]1[C:9]([CH3:19])=[C:10]([C:15]([F:18])=[CH:16][CH:17]=1)[C:11]([O:13][CH3:14])=[O:12])(C)(C)C.CC(C)([O-])C.[K+]>CS(C)=O.O>[F:18][C:15]1[CH:16]=[CH:17][C:8]2[C:9](=[CH:19][NH:6][N:7]=2)[C:10]=1[C:11]([O:13][CH3:14])=[O:12]

참가 물질

5

반응물 2

HCID 23665647Potassium tert-butoxideHCID 59334531Methyl 3-[(tert-butylthio)diazenyl]-6-fluoro-2-methylbenzoate

생성물 1

HCID 178498690HCID 178498690, 화합물수율 25.3%

시약·촉매·용매 2

HCID 679Dimethyl Sulfoxide용매2회HCID 962Water용매

실험 절차

To a solution of a crudely purified product (18.5 g, 65.1 mmol) of methyl 3-[(tert-butylthio)diazenyl]-6-fluoro-2-methylbenzoate in dimethyl sulfoxide (200 mL) was added a solution of potassium tert-butoxide (10.6 g, 98.0 mmol) in dimethyl sulfoxide (125 mL) at room temperature, and the mixture was stirred for 12 hr. The reaction solution was diluted with water, and the mixture was extracted with ethyl acetate. The extract was washed with saturated brine, and 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 (3.20 g, yield 25%).

후처리

  1. extractionthe mixture was extracted with ethyl acetate
  2. washThe extract was washed with saturated brine
  3. dry with materialdried 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-d94e5e979edb478583cce5b6762217a9
출처 데이터셋
uspto-grants-2012_02
특허 번호
US08110585B2

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