Ethyl Acetate → 1-(Methylsulfonyl)-4-nitrobenzene

HRID 1883001ノート

反応式

HRID 1883001 の反応式
[N+:1]([C:4]1[CH:9]=[CH:8][C:7](SC)=[CH:6][CH:5]=1)([O-:3])=[O:2].Cl[C:13]1C=C(C=CC=1)C(OO)=O.C(OCC)(=O)C.[S:29](=[O:32])(O)[O-:30].[Na+]>C(Cl)(Cl)Cl>[CH3:13][S:29]([C:7]1[CH:8]=[CH:9][C:4]([N+:1]([O-:3])=[O:2])=[CH:5][CH:6]=1)(=[O:32])=[O:30]

参加物

6

反応物 4

HCID 8857Ethyl AcetateHCID 70297m-Chloroperbenzoic acidHCID 961094-Nitrophenyl methyl sulfideHCID 23665763Sodium Bisulfite

生成物 1

HCID 2584341-(Methylsulfonyl)-4-nitrobenzene収率 95%

試薬・触媒・溶媒 1

HCID 6212Chloroform溶媒

実験手順

To a stirring solution of methyl 4-nitrophenyl sulfide (10 g, 59.1 mmol) in chloroform at 0° C. was added m-chloroperoxybenzoic acid (55.6 g, 177.3 mmol). After 3 h, ethyl acetate (1.2 L) was added followed by satd aq sodium bisulfite. After stirring overnight, the layers were separated and the organic phase was washed with satd ag sodium bicarbonate (3×200 mL), followed by brine, and then dried over MgSO4, filtered and concentrated in vacuo to give 11.27 g (95%) of the title compound.

後処理

  1. customthe layers were separated
  2. washthe organic phase was washed with satd ag sodium bicarbonate (3×200 mL)
  3. dry with materialdried over MgSO4
  4. filtrationfiltered
  5. concentrationconcentrated in vacuo

出典と根拠

ORDレコード
ord-c03962031ef34e7a8baf52c5bfdf2470
出典データセット
uspto-grants-2004_07
特許番号
US06759414B2

反応ノート

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