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

HRID 988669노트

반응식

HRID 988669 반응식
[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]

참가 물질

6

반응물 4

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

생성물 1

HCID 2584341-(Methylsulfonyl)-4-nitrobenzene수율 95%

시약·촉매·용매 1

HCID 6212Chloroform용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-f0d65ff0dffa4a90b93f89a3cf48e3e1
출처 데이터셋
uspto-grants-2003_10
특허 번호
US06635657B1

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