Potassium tert-butoxide → HCID 178498690、化合物

HRID 1639777ノート

反応式

HRID 1639777 の反応式
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]

参加物

5

反応物 2

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

生成物 1

HCID 178498690HCID 178498690、化合物収率 25.3%

試薬・触媒・溶媒 2

HCID 679Dimethyl Sulfoxide溶媒2 回HCID 962Water溶媒

実験手順

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%).

後処理

  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)

出典と根拠

ORDレコード
ord-d94e5e979edb478583cce5b6762217a9
出典データセット
uspto-grants-2012_02
特許番号
US08110585B2

反応ノート

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