Sodium Hydroxide → 4(Fluoromethyl-ethyl)-nitrobenzene

HRID 1379972노트

반응식

HRID 1379972 반응식
[F:1][CH2:2][C:3]([C:5]1[CH:10]=[CH:9][C:8]([N+:11]([O-:13])=[O:12])=[CH:7][CH:6]=1)=[CH2:4].NOS(O)(=O)=O.S(O)(O)(=O)=O.NO.[OH-].[Na+]>CO>[F:1][CH2:2][CH:3]([C:5]1[CH:10]=[CH:9][C:8]([N+:11]([O-:13])=[O:12])=[CH:7][CH:6]=1)[CH3:4]

참가 물질

6

반응물 4

HCID 14798Sodium HydroxideHCID 76284hydroxylamine-O-sulfonic acidHCID 159255Hydroxylamine, sulfate (1:1)HCID 13187365HCID 13187365, 화합물

생성물 1

HCID 131873674(Fluoromethyl-ethyl)-nitrobenzene

시약·촉매·용매 1

HCID 887Methanol용매2회

실험 절차

To a solution of 17.5 g (0.1 Mol) 4(1-fluoromethylethenyl)-nitrobenzene in 400 ml CH3OH are added 100 g (0.8 Mol) 90% hydroxylamine-O-sulphonic acid and 67.2 g (0.41 Mol) hydroxylamine sulphate. The reaction mixture is then rendered alkaline (pH 8) at 15°-20° cooling with ice water) with 20% aqueous NaOH. After the addition of a further 500 ml portion of CH3OH the reaction mixture is stirred at room temperature for 24 hours, and then filtered. The filtrate is evaporated in vacuo. The residue is dissolved in CH2Cl2, this solution washed with H2O, dried over Na2SO4 and evaporated. The light yellow, chromatographically (this layer) pure liquid (Rf=0.5; CHCl3 /CCl4 1:1 on silica gel) is vaccum distilled, to give the title compound, b.p. 103°-104°/0.1 Torr.

후처리

  1. customat 15°-20°
  2. filtrationfiltered
  3. customThe filtrate is evaporated in vacuo
  4. dissolutionThe residue is dissolved in CH2Cl2
  5. washthis solution washed with H2O
  6. dry with materialdried over Na2SO4
  7. customevaporated

출처 및 근거

ORD 기록
ord-a5bdf1b79488423f819e11151df83b62
출처 데이터셋
uspto-grants-1986_04
특허 번호
US04579585

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