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

HRID 988669ノート

反応式

HRID 988669 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 aq 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 aq 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-f0d65ff0dffa4a90b93f89a3cf48e3e1
出典データセット
uspto-grants-2003_10
特許番号
US06635657B1

反応ノート

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