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Methanesulfonamide → N-(Diphenoxymethylene)-methanesulfonamide

HRID 1869002
ノート
印刷プレビュー

反応式

HRID 1869002 の反応式
Cl[CH:2](Cl)[O:3][C:4]1[CH:9]=[CH:8][CH:7]=[CH:6][CH:5]=1.[CH3:11][S:12]([NH2:15])(=[O:14])=[O:13].[C:16](=[O:19])([O-])O.[Na+]>C(#N)C>[CH3:11][S:12]([N:15]=[C:2]([O:19][C:16]1[CH:8]=[CH:9][CH:4]=[CH:5][CH:6]=1)[O:3][C:4]1[CH:9]=[CH:8][CH:7]=[CH:6][CH:5]=1)(=[O:14])=[O:13]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 72879MethanesulfonamideHCID 319898Dichloromethyl phenyl etherHCID 516892Sodium Bicarbonate

生成物 1

HCID 13738851N-(Diphenoxymethylene)-methanesulfonamide

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

実験手順

To a solution of dichlorophenoxymethane (1 g) in acetonitrile (10 mL) was added methanesulfonamide (0.39 g) under ice-cooling, and the mixture was stirred at room temperature for 48 hours. The reaction mixture was poured into a saturated aqueous sodium hydrogen carbonate solution, and the resuling mixture was extracted with ethyl acetate. The organic layer was washed with water and brine, and dried over anhydrous magnesium sulfate. The solvent was removed under reduced pressure to give 1-(N-methanesulfonylimino)-1,1-diphenoxymethane (0.95 g). To a solution of 3-(2,3,4,6-tetra-O-acetyl-β-D-glucopyranosyloxy)-4-{[4-(2-aminoethoxy)-2-methylphenyl]methyl}-5-isopropyl-1H-pyrazole (50 mg) in tetrahydrofuran (1 mL) was added 1-(N-methanesulfonylimino)-1,1-diphenoxymethane (26 mg) under ice-cooling, and the mixture was stirred at room temperature for 1 hour. To the reaction mixture was added 2-aminoethanol (49 mg), and the mixture was stirred at 60° C. overnight. The reaction mixture was concentrated under reduced pressure, and the residue was dissolved in methanol (2 mL). To the solution was added sodium methoxide (28% methanol solution, 0.008 mL), and the mixture was stirred at room temperature for 3 hours. To the reaction mixture was added acetic acid (0.01 mL). The resulting mixture was concentrated under reduced pressure, and the residue was purified by solid phase extraction on ODS (washing solvent: distilled water, eluent: methanol) to give the title compound (38 mg).

後処理

  1. temperaturecooling
  2. extractionthe resuling mixture was extracted with ethyl acetate
  3. washThe organic layer was washed with water and brine
  4. dry with materialdried over anhydrous magnesium sulfate
  5. customThe solvent was removed under reduced pressure

出典と根拠

ORDレコード
ord-959fc890e162467c8959545ecc6bde8b
出典データセット
uspto-grants-2009_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07635684B2

反応ノート

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